This document describes a study that developed a simple, selective, accurate, and low-cost spectrophotometric method for determining satranidazole content in bulk drugs and pharmaceutical formulations. The method involves forming an ion-association complex between satranidazole and the acidic dye Tropaeolin OOO that is extractable in chloroform. The extracted colored complex has maximum absorbance at 484 nm and follows Beer's law within the concentration range of 4-20 μg/mL. The method was validated according to ICH guidelines and demonstrated high accuracy and precision for quantifying satranidazole in commercial drug products.
Spectrophotometric Determination of Drugs and Pharmaceuticals by Cerium (IV) ...IOSR Journals
Simple, sensitive, accurate, and precise spectrophotometric methods for quantitative determination of drugs, viz., Darifenacin (DAR), Esmolol Hydrochloride (ESM), Montelukast Sodium (MON), Sildenafil citrate (SIL),Terbinafine (TER) and Tramadol Hydrochloride (TRA) were developed. The method of each drug depends upon oxidation of drugs by Ce (IV) (Excess) and estimating the amount of unreacted Ce (IV) by amaranth dye at 523nm. The calibration curves obeyed Beer’s law over the concentration range of 1.4-7.0 μg ml-1 (DAR), 2-14 μg ml-1 (ESM), 2-10 μg ml-1 (MON), 20-70 μg ml-1 (SIL), 3-21 μg ml-1 (TER) & 2-14 μg ml-1 (TRA). The methods have been validated in terms of guidelines of ICH and applied to analysis of pharmaceuticals.
Development and Validation of the HPLC Method for the Analysis of Ametridio...iosrphr_editor
The IOSR Journal of Pharmacy (IOSRPHR) is an open access online & offline peer reviewed international journal, which publishes innovative research papers, reviews, mini-reviews, short communications and notes dealing with Pharmaceutical Sciences( Pharmaceutical Technology, Pharmaceutics, Biopharmaceutics, Pharmacokinetics, Pharmaceutical/Medicinal Chemistry, Computational Chemistry and Molecular Drug Design, Pharmacognosy & Phytochemistry, Pharmacology, Pharmaceutical Analysis, Pharmacy Practice, Clinical and Hospital Pharmacy, Cell Biology, Genomics and Proteomics, Pharmacogenomics, Bioinformatics and Biotechnology of Pharmaceutical Interest........more details on Aim & Scope).
Method Development and Validation of Clopidogrel Bisulphate by Reverse Phase-...SriramNagarajan15
A new, simple sensitive, rapid, accurate and precise RP-HPLC method was developed for the estimation of Clopidogrel bisulphate in bulk drug and pharmaceutical formulation. Clopidogrel bisulphate was chromatographed on a reverse phase C18column (150 mm x 4.5 mm, i.d 5μm) in a mobile phase consisting of acetonitrile and phosphate buffer (pH: 3.0) in the ratio of 60:40 % v/v. The mobile phase was pumped at a flow rate of 1 ml/min with detection at 224 nm. The detector response was linear in the concentration of 50-150 μg /ml. The limit of detection and limit of quantitation was found to be 1.3 and 4.2 µg/ml, respectively. The intra and inter day variation was found to be less than 2%. The mean recovery of the drug from the solution was 99.79%. The proposed method is simple, fast, accurate, precise and reproducible hence, it can be applied for routine quality control analysis of Clopidogrel bisulphate in bulk drug and pharmaceutical formulation. Key words: Clopidogrel bisulphate, RP-HPLC, Validation, Accuracy, Precision.
Notes* for the subject 'Advanced Pharmaceutical Analysis'Sanathoiba Singha
As per the syllabus prescribed by Rajiv Gandhi University of Health Sciences, Karnataka, for M. Pharm (Pharmaceutical Analysis) 1st semester.
*not all topics have been included in this collection of notes.
DETERMINATION OF MIANSERIN USING TROPAEOLIN-OOO BY ION PAIR FORMATIONRatnakaram Venkata Nadh
Objective: The present study was aimed at the development of a simple visible spectrophotometric method for the assay of mianserin, a drug used for the treatment of depression.
Methods: The method was developed using tropaeolin-ooo (TPooo) as an ion associative complex forming a chromophore. Developed the chromophore by sequential mixing of aqueous solutions of mianserin, hydrochloric acid, and TPooo. Chromophore was extracted into an organic solvent (chloroform) and absorbance values of organic layers were measured. As per the existing guidelines of an international conference on harmonization (ICH), various parameters of the method were tested for validation.
Results: At the optimized reaction conditions, the formed chromophore (λ max
Conclusion: Due to lack of pre-treatment process for this method, it was simple. All the tested parameters of the method were validated as per ICH guidelines.
Spectrophotometric Determination of Drugs and Pharmaceuticals by Cerium (IV) ...IOSR Journals
Simple, sensitive, accurate, and precise spectrophotometric methods for quantitative determination of drugs, viz., Darifenacin (DAR), Esmolol Hydrochloride (ESM), Montelukast Sodium (MON), Sildenafil citrate (SIL),Terbinafine (TER) and Tramadol Hydrochloride (TRA) were developed. The method of each drug depends upon oxidation of drugs by Ce (IV) (Excess) and estimating the amount of unreacted Ce (IV) by amaranth dye at 523nm. The calibration curves obeyed Beer’s law over the concentration range of 1.4-7.0 μg ml-1 (DAR), 2-14 μg ml-1 (ESM), 2-10 μg ml-1 (MON), 20-70 μg ml-1 (SIL), 3-21 μg ml-1 (TER) & 2-14 μg ml-1 (TRA). The methods have been validated in terms of guidelines of ICH and applied to analysis of pharmaceuticals.
Development and Validation of the HPLC Method for the Analysis of Ametridio...iosrphr_editor
The IOSR Journal of Pharmacy (IOSRPHR) is an open access online & offline peer reviewed international journal, which publishes innovative research papers, reviews, mini-reviews, short communications and notes dealing with Pharmaceutical Sciences( Pharmaceutical Technology, Pharmaceutics, Biopharmaceutics, Pharmacokinetics, Pharmaceutical/Medicinal Chemistry, Computational Chemistry and Molecular Drug Design, Pharmacognosy & Phytochemistry, Pharmacology, Pharmaceutical Analysis, Pharmacy Practice, Clinical and Hospital Pharmacy, Cell Biology, Genomics and Proteomics, Pharmacogenomics, Bioinformatics and Biotechnology of Pharmaceutical Interest........more details on Aim & Scope).
Method Development and Validation of Clopidogrel Bisulphate by Reverse Phase-...SriramNagarajan15
A new, simple sensitive, rapid, accurate and precise RP-HPLC method was developed for the estimation of Clopidogrel bisulphate in bulk drug and pharmaceutical formulation. Clopidogrel bisulphate was chromatographed on a reverse phase C18column (150 mm x 4.5 mm, i.d 5μm) in a mobile phase consisting of acetonitrile and phosphate buffer (pH: 3.0) in the ratio of 60:40 % v/v. The mobile phase was pumped at a flow rate of 1 ml/min with detection at 224 nm. The detector response was linear in the concentration of 50-150 μg /ml. The limit of detection and limit of quantitation was found to be 1.3 and 4.2 µg/ml, respectively. The intra and inter day variation was found to be less than 2%. The mean recovery of the drug from the solution was 99.79%. The proposed method is simple, fast, accurate, precise and reproducible hence, it can be applied for routine quality control analysis of Clopidogrel bisulphate in bulk drug and pharmaceutical formulation. Key words: Clopidogrel bisulphate, RP-HPLC, Validation, Accuracy, Precision.
Notes* for the subject 'Advanced Pharmaceutical Analysis'Sanathoiba Singha
As per the syllabus prescribed by Rajiv Gandhi University of Health Sciences, Karnataka, for M. Pharm (Pharmaceutical Analysis) 1st semester.
*not all topics have been included in this collection of notes.
DETERMINATION OF MIANSERIN USING TROPAEOLIN-OOO BY ION PAIR FORMATIONRatnakaram Venkata Nadh
Objective: The present study was aimed at the development of a simple visible spectrophotometric method for the assay of mianserin, a drug used for the treatment of depression.
Methods: The method was developed using tropaeolin-ooo (TPooo) as an ion associative complex forming a chromophore. Developed the chromophore by sequential mixing of aqueous solutions of mianserin, hydrochloric acid, and TPooo. Chromophore was extracted into an organic solvent (chloroform) and absorbance values of organic layers were measured. As per the existing guidelines of an international conference on harmonization (ICH), various parameters of the method were tested for validation.
Results: At the optimized reaction conditions, the formed chromophore (λ max
Conclusion: Due to lack of pre-treatment process for this method, it was simple. All the tested parameters of the method were validated as per ICH guidelines.
Natural Anthraquinone Synthesis and DART-MS Analysis/DatabasingSteven Augustin
Poster Presentation at 2015 Great Lakes and Central Region Joint Meeting of the American Chemical Society. Eastern Michigan University Graduate Research, Dr. Ruth Ann Armitage and Dr. Timothy Friebe, graduate advisers.
Ion-pair Formation for the Determination of Mianserin Using Fast Sulphon Black FRatnakaram Venkata Nadh
Aim: The objective of the current study is to develop a colorimetric method for the determination of mianserin, an antidepressant drug. Materials and Methods: Fast Sulphon Black F, an acidic dye was used to develop a soluble colored ion-pair complex. The complex was extracted into an organic solvent and absorbance was measured. Results: Reaction conditions were optimized to obtain a sensitive and stable chromophore (λmax 554 nm) in dichloromethane. Good linearity was observed for the calibration curve plotted in the studied concentration range (4–14 μg/mL) with regression analysis (r > 0.9997). High percentage recovery values (98.25–101.40) show that the method is accurate. Reproducibility of the method is evident from lower relative standard deviation (<2%) for both intra- and inter-day precision studies. Conclusions: The proposed method is validated as per the existing ICH guidelines. This method is simple as it does not require any pre-treatment process.
Development and Validation of Reversed-phase High-performance Liquid Chromato...BRNSS Publication Hub
A new, reliable, and sensitive reversed-phase high-performance liquid chromatography method has been developed and validated for simultaneous assay of benzoyl peroxide (BPO) and resveratrol. An isocratic separation of BPO and resveratrol was achieved on C18, 250 mm × 4.6 mm I.d., 5 μm particle size columns with a flow rate of 1.2 ml/min and using a UV detector to monitor the elute at 245 nm. The mobile phase consisted of an ammonium acetate (pH 4) and ethanol. Response was a linear function of drug concentration in the range of 10–100 mg/mL range with an R2 of 0.993 for BPO and 10–100 μg/mL range with an R2 of 0.995 for resveratrol, accuracy with percent relative standard deviation of 100.65 ± 0.23 (benzoic peroxide) and 100.48 ± 0.45 (resveratrol) and with a limit of detection and quantification for BPO and resveratrol, respectively. The result of analysis has been validated statistically and by recovery study. The accuracy ranged between 99.65 and 101.91%. The method was found to be precise, reproducible, and rapid.
New RP HPLC method for the estimation of imatinib in pharmaceutical dosage formSriramNagarajan19
A simple and selective LC method is described for the determination of Imatinib dosage forms. Chromatographic separation was achieved on a c18 column using mobile phase consisting of a mixture of Water: Acetonitrile (30:70 v/v), with detection of 272nm. Linearity was observed in the range 50-150 µg /ml for Imatinib (r2 =0.9976) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.
Diazo coupling for the determination of selexipag by visible spectrophotometryRatnakaram Venkata Nadh
Aim and Objective: The aim and objective of this study were to develop a spectrophotometric method for the assay of selexipag (selective IP prostacyclin receptor agonist indicated for the treatment of pulmonary arterial hypertension) in pure and pharmaceutical formulations so that it will be an alternative quantitative method to chromatographic methods which require large quantities of organic solvents, where some are with hazardous and toxic properties. Materials and Methods: The method is based on the diazo coupling of selexipag with diazotized p-nitroaniline in alkaline medium to form a stable green-colored and water-soluble azo dye with a maximum absorption at 510 nm. Optimization of reaction conditions was carried out to get highly sensitive and stable colored complex. Results and Discussion: Beer’s law is obeyed over the concentration range of 2–12 μg/mL with a molar absorptivity of 3.33 × 104 L/mol/cm. The limit of detection was 0.35 μg/mL and limit of quantification was 1.0 μg/mL. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%). Conclusions: This method was tested and validated for various parameters according to the current ICH guidelines.
DETERMINATION OF MIANSERIN USING TROPAEOLIN-OOO BY ION PAIR FORMATIONRatnakaram Venkata Nadh
Objective: The present study was aimed at the development of a simple visible spectrophotometric method for the assay of mianserin, a drug used for the treatment of depression.
Methods: The method was developed using tropaeolin-ooo (TPooo) as an ion associative complex forming a chromophore. Developed the chromophore by sequential mixing of aqueous solutions of mianserin, hydrochloric acid, and TPooo. Chromophore was extracted into an organic solvent (chloroform) and absorbance values of organic layers were measured. As per the existing guidelines of an international conference on harmonization (ICH), various parameters of the method were tested for validation.
Results: At the optimized reaction conditions, the formed chromophore (λ max
Conclusion: Due to lack of pre-treatment process for this method, it was simple. All the tested parameters of the method were validated as per ICH guidelines.
Analytical method development and validation for the estimation of quinapril ...SriramNagarajan19
A simple and selective LC method is described for the determination of Quinapril and Tolcapone tablet dosage forms. Chromatographic separation was achieved on a c18 column using mobile phase consisting of a Mixed Phosphate buffer (KH2PO4 +K2HPO4): Acetonitrile 40:60, with detection of 239 nm. Linearity was observed in the range 50 - 150 µg /ml for Quinapril (r2 =0.995) and 62.5- 187.5µg /ml for Tolcapone (r2 =0.999) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim.
The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.
International Journal of Pharmaceutical Science Invention (IJPSI) is an international journal intended for professionals and researchers in all fields of Pahrmaceutical Science. IJPSI publishes research articles and reviews within the whole field Pharmacy and Pharmaceutical Science, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
STUDIES ON TREATMENT OF PHARMACEUTICAL WASTE EFFLUENTS BY POLYMER MATERIALS M...EDITOR IJCRCPS
In the present study, sorption technique was used to achieve the optimum recovery of the pharmaceutical waste from effluents.
The modified urea formaldehyde resin was prepared and mixed with inorganic adsorbent at various proportions. The removal
capabilities of pharmaceutical waste by the prepared composite materials were investigated. Different factors affecting the uptake
such as contact time, pH value and aqueous volume to resin weight ratio have been investigated. The reaction mechanisms and
the optimum conditions for the treatment were deduced in the light of the obtained results.
Keywords: Sorption technique, Pharmaceutical waste, Different factors.
Natural Anthraquinone Synthesis and DART-MS Analysis/DatabasingSteven Augustin
Poster Presentation at 2015 Great Lakes and Central Region Joint Meeting of the American Chemical Society. Eastern Michigan University Graduate Research, Dr. Ruth Ann Armitage and Dr. Timothy Friebe, graduate advisers.
Ion-pair Formation for the Determination of Mianserin Using Fast Sulphon Black FRatnakaram Venkata Nadh
Aim: The objective of the current study is to develop a colorimetric method for the determination of mianserin, an antidepressant drug. Materials and Methods: Fast Sulphon Black F, an acidic dye was used to develop a soluble colored ion-pair complex. The complex was extracted into an organic solvent and absorbance was measured. Results: Reaction conditions were optimized to obtain a sensitive and stable chromophore (λmax 554 nm) in dichloromethane. Good linearity was observed for the calibration curve plotted in the studied concentration range (4–14 μg/mL) with regression analysis (r > 0.9997). High percentage recovery values (98.25–101.40) show that the method is accurate. Reproducibility of the method is evident from lower relative standard deviation (<2%) for both intra- and inter-day precision studies. Conclusions: The proposed method is validated as per the existing ICH guidelines. This method is simple as it does not require any pre-treatment process.
Development and Validation of Reversed-phase High-performance Liquid Chromato...BRNSS Publication Hub
A new, reliable, and sensitive reversed-phase high-performance liquid chromatography method has been developed and validated for simultaneous assay of benzoyl peroxide (BPO) and resveratrol. An isocratic separation of BPO and resveratrol was achieved on C18, 250 mm × 4.6 mm I.d., 5 μm particle size columns with a flow rate of 1.2 ml/min and using a UV detector to monitor the elute at 245 nm. The mobile phase consisted of an ammonium acetate (pH 4) and ethanol. Response was a linear function of drug concentration in the range of 10–100 mg/mL range with an R2 of 0.993 for BPO and 10–100 μg/mL range with an R2 of 0.995 for resveratrol, accuracy with percent relative standard deviation of 100.65 ± 0.23 (benzoic peroxide) and 100.48 ± 0.45 (resveratrol) and with a limit of detection and quantification for BPO and resveratrol, respectively. The result of analysis has been validated statistically and by recovery study. The accuracy ranged between 99.65 and 101.91%. The method was found to be precise, reproducible, and rapid.
New RP HPLC method for the estimation of imatinib in pharmaceutical dosage formSriramNagarajan19
A simple and selective LC method is described for the determination of Imatinib dosage forms. Chromatographic separation was achieved on a c18 column using mobile phase consisting of a mixture of Water: Acetonitrile (30:70 v/v), with detection of 272nm. Linearity was observed in the range 50-150 µg /ml for Imatinib (r2 =0.9976) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.
Diazo coupling for the determination of selexipag by visible spectrophotometryRatnakaram Venkata Nadh
Aim and Objective: The aim and objective of this study were to develop a spectrophotometric method for the assay of selexipag (selective IP prostacyclin receptor agonist indicated for the treatment of pulmonary arterial hypertension) in pure and pharmaceutical formulations so that it will be an alternative quantitative method to chromatographic methods which require large quantities of organic solvents, where some are with hazardous and toxic properties. Materials and Methods: The method is based on the diazo coupling of selexipag with diazotized p-nitroaniline in alkaline medium to form a stable green-colored and water-soluble azo dye with a maximum absorption at 510 nm. Optimization of reaction conditions was carried out to get highly sensitive and stable colored complex. Results and Discussion: Beer’s law is obeyed over the concentration range of 2–12 μg/mL with a molar absorptivity of 3.33 × 104 L/mol/cm. The limit of detection was 0.35 μg/mL and limit of quantification was 1.0 μg/mL. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%). Conclusions: This method was tested and validated for various parameters according to the current ICH guidelines.
DETERMINATION OF MIANSERIN USING TROPAEOLIN-OOO BY ION PAIR FORMATIONRatnakaram Venkata Nadh
Objective: The present study was aimed at the development of a simple visible spectrophotometric method for the assay of mianserin, a drug used for the treatment of depression.
Methods: The method was developed using tropaeolin-ooo (TPooo) as an ion associative complex forming a chromophore. Developed the chromophore by sequential mixing of aqueous solutions of mianserin, hydrochloric acid, and TPooo. Chromophore was extracted into an organic solvent (chloroform) and absorbance values of organic layers were measured. As per the existing guidelines of an international conference on harmonization (ICH), various parameters of the method were tested for validation.
Results: At the optimized reaction conditions, the formed chromophore (λ max
Conclusion: Due to lack of pre-treatment process for this method, it was simple. All the tested parameters of the method were validated as per ICH guidelines.
Analytical method development and validation for the estimation of quinapril ...SriramNagarajan19
A simple and selective LC method is described for the determination of Quinapril and Tolcapone tablet dosage forms. Chromatographic separation was achieved on a c18 column using mobile phase consisting of a Mixed Phosphate buffer (KH2PO4 +K2HPO4): Acetonitrile 40:60, with detection of 239 nm. Linearity was observed in the range 50 - 150 µg /ml for Quinapril (r2 =0.995) and 62.5- 187.5µg /ml for Tolcapone (r2 =0.999) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim.
The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.
International Journal of Pharmaceutical Science Invention (IJPSI) is an international journal intended for professionals and researchers in all fields of Pahrmaceutical Science. IJPSI publishes research articles and reviews within the whole field Pharmacy and Pharmaceutical Science, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
STUDIES ON TREATMENT OF PHARMACEUTICAL WASTE EFFLUENTS BY POLYMER MATERIALS M...EDITOR IJCRCPS
In the present study, sorption technique was used to achieve the optimum recovery of the pharmaceutical waste from effluents.
The modified urea formaldehyde resin was prepared and mixed with inorganic adsorbent at various proportions. The removal
capabilities of pharmaceutical waste by the prepared composite materials were investigated. Different factors affecting the uptake
such as contact time, pH value and aqueous volume to resin weight ratio have been investigated. The reaction mechanisms and
the optimum conditions for the treatment were deduced in the light of the obtained results.
Keywords: Sorption technique, Pharmaceutical waste, Different factors.
New RP HPLC method for the simultaneous estimation of sulbactum and ceftriaxo...SriramNagarajan19
A simple and selective LC method is described for the determination of Sulbactum and Ceftriaxone tablet dosage forms. Chromatographic separation was achieved on a C18 column using mobile phase consisting of a mixture of mixture of 60 volumes of 20mM Phosphate buffer pH 3.5: 40 volumes of Acetonitrile (60:40 v/v) with detection of 210 nm. Linearity was observed in the range 30-70 µg /ml for Sulbactum (r2 =0.9998) and 60-140µg /ml for Ceftriaxone (r2 =0.9983) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.
A STUDY ON FORMATION OF SALYCILIC ACID FORMALDEHYDE POLYMER SAMPLEEDITOR IJCRCPS
Condensation of salicylic acid (0.02 mole) with formaldehyde (0.016 mole) in presence of aqueous 40% H2SO4.
Keywords: pipette,thermometer,spectro-photometer,conicalflakk,waterbath.
Stability indicating method development and validation for the estimation of ...SriramNagarajan18
Stability indicating method development and validation for the estimation of Doxorubicin by using RP-HPLC method in a bulk and pharmaceutical dosage form
COMPARATIVE INVESTIGATION OF FOOD SUPPLEMENTS
CONTAINING ASCORBIC ACID
Danka Obreshkova and Boyka Tsvetkova
Medical University – Sofia, Faculty of Pharmacy, Dept. of Pharmaceutical chemistry
Abstract. A simple, specific, precise and accurate reversed phase liquid chromatographic (RP-LC) method
has been developed for the determination of ascorbic acid in different food additives. The chromatographic
separation was achieved on a LiChrosorb C18, 250 mm x 4.6 mm, 5 μm column at a detector wavelength
of 230 nm and a flow rate of 1.5 ml/min. The mobile phase was composed of acetonitrile and water (60:40
v/v). The retention time of analyte was 3.49 min. The method was validated for the parameters like specificity,
linearity, precision, accuracy, limit of quantitation and limit of detection. The method was found to be
specific as no other peaks of impurities and excipients were observed. The square of correlation coefficient
(R2) was 0.9997 while relative standard deviations were found to be <2.0%. The proposed RP-LC method
can be applied for the routine analysis of commercially available food additives of ascorbic acid.
Ceftriaxone is one of the third generations of cephalosporin antibiotics and commercially found as a sodium salt. The market demand for it is still high in recent years, including in Indonesia. However, there is no local production manufacture yet. A high yield of ceftriaxone sodium would be an advantage in industrial scale. Ceftriaxone was synthesized by reacting 7–amino–3–[(2,5–dihydro–6–hydroxy–2–methyl–5–oxo–1,2,4–triazin–3–yl) thiomethyl] cephalosporanic acid (7-ACT) with 2-Mercaptobenzothiazolyl (Z)-2-(2-Aminothiazole-4-yl)-2-Methoxyimino Acetate (MAEM) then with sodium salt in basic condition. The product was generated by solventing-out using acetone. The products were analyzed by HPLC quantitatively and the structure was confirmed using FTIR, MS and NMR. In this research, the variation in the mole ratio of reactants against the yield of product was evaluated. The result showed that the variations in mole ratio reactants affect the yield production. The higher ratio of MAEM would be the higher yield is obtained. The results show that the yield was 72,17% at mole ratio 1:2 which has 99,32% purity. This result could be a consideration in industrial production scale in ceftriaxone sodium preparation.
Synthesis, Characterization and Biological Evaluation of Oxazolone Derivativesijceronline
A series of six 4-aryl Benzelidene-2-phenyl-5- oxazolone derivatives were synthesized by condensation of aromatic aldehydes with N-benzoyl glycine (Hippuric acid) in the presence of sodium acetate and acetic anhydride at room temperature in ethanol. Six of the compounds are new derivatives. The structures of the compounds were evaluated based on 1H-NMR , IR and FTIR methods and by elemental analysis. .All the derivative compounds prepared were tested for their antimicrobial activity by disk diffusion technique. Test organisms: Bacteria like Staphylococcus aureusMTCC 7443 and Salmonella typhimuriumMTCC 733 Fungi like C.albicans and A.flavus The results were compared with those of the standard 0.5% Ciprofloxacin. The derivatives with Salicylaldehyde and cinnamaldehyde were showed excellent activities against E. coli. and Staphylococcus aureusMTCC 7443 : than Salmonella typhimuriumMTCC 733 bacteria. It also showed reasonable activity withFungi like C.albicans than A.flavus
Quality-by-design-based development and validation of a stability-indicating ...Ratnakaram Venkata Nadh
A systematic design-of-experiments was performed by applying quality-by-design concepts to determine
design space for rapid quantification of teriflunomide by the ultraperformance liquid chromatography
(UPLC) method in the presence of degradation products. Response surface and central composite
quadratic were used for statistical evaluation of experimental data using a Design-Expert software. The
response variables such as resolution, retention time, and peak tailing were analyzed statistically for the
screening of suitable chromatographic conditions. During this process, various plots such as perturbation,
contour, 3D, and design space were studied. The method was developed through UPLC BEH C18
2.1 � 100 mm, 1.7-μ column, mobile phase comprised of buffer (5 mM K2HPO4 containing 0.1%
triethylamine, pH 6.8), and acetonitrile (40:60 v/v), the flow rate of 0.5 mL min 1 and UV detection at
250 nm. The method was developed with a short run time of 1 min. Forced degradation studies revealed
that the method was stability-indicating, suitable for both assay and in-vitro dissolution of a drug product.
The method was found to be linear in the range of 28–84 μg mL 1, 2.8–22.7 μg mL 1 with a correlation
coefficient of 0.9999 and 1.000 for assay and dissolution, respectively. The recovery values were found in
the range of 100.1–101.7%. The method was validated according to ICH guidelines.
Electrochemical study of anatase TiO2 in aqueous sodium-ion electrolytesRatnakaram Venkata Nadh
In this paper, a basic electro-analytical study on the behavior of anatase TiO2 in aqueous NaOH has been presented using cyclic voltammetry technique (CV). The study has explored the possibility of using TiO2 as anode material for ARSBs in presence of 5 M NaOH aqueous electrolyte. CV profiles show that anatase TiO2 exhibits reversible sodium ion insertion/de-insertion reactions. CV studies of TiO2 anode in aqueous sodium electrolytes at different scan rate shows that the Na+ ion insertion reaction at the electrode is diffusion controlled with a resistive behavior. Proton insertion from aqueous sodium electrolytes into TiO2 cannot be ruled out. To confirm the ion inserted and de-inserted, CV studies are done at different concentration of NaOH and it is found that at lower concentrations of NaOH, proton insertion process competes with Na+ ion insertion process and as the concentration increases, the Na+ ion insertion process becomes the predominant electrode reaction making it suitable anode materials for aqueous sodium batteries in 5 M NaOH.
Validated HPLC Method for Assay and Content Uniformity Testing of Roflumilast...Ratnakaram Venkata Nadh
Roflumilast is a selective enzyme inhibitor of phosphodiesterase-4. This drug is recommended for treatment of patients suffering from
chronic-obstructive-pulmonary-disease with chronic-bronchitis. Roflumilast is not official in pharmacopoeia and the reported methods
are having high chromatographic run times. A short run time HPLC method was developed for assay and content uniformity testing to
determine the roflumilast in blend and tablets. The mobile phase consists of 10 mM sodium dihydrogen phosphate monohydrate buffer
and acetonitrile in the ratio of 45:55 v/v. The HPLC method was developed using accucore-C18 150 × 4.6 mm, 4 μm column with a flow
rate of 1.0 mL min-1, 215 nm wavelength and 10 μL injection volume with run time of 5 min. The method linearity was proved between
5.02-40.17 μg mL-1 and obtained correlation-coefficient value is 1.0000. The mean recovery of roflumilast was 100.6%. The stability
indicating nature was established and performed the validation by considering ICH Q2 (R1) recommendations.
Substrate Inhibition in Ruthenium(III) Catalyzed Oxidation of Propane-1,3-dio...Ratnakaram Venkata Nadh
Ruthenium(III) catalyzed oxidation of propane-1,3-diol by potassium periodate was studied in aqueous perchloric acid medium. Orders
of reaction with respect to concentrations of oxidant, substrate, acid and catalyst were determined. First order in oxidant and catalyst
concentrations, and inverse fractional order in acid medium were observed. In addition, substrate inhibition (i.e. a decrease in reaction rate
with an increase in substrate concentration) was observed. Effect of addition of salt and solvent was studied. Based on the studies of
temperature variation, Arrhenius parameters were calculated. Plausible mechanism was also proposed based on observed kinetics.
Ruthenium(III) Catalyzed Oxidation of Sugar Alcohols by Dichloroisocyanuric A...Ratnakaram Venkata Nadh
Kinetics of ruthenium(III) catalyzed oxidation of biologically important sugar alcohols (myo-inositol,
D-sorbitol, and D-mannitol) by dichloroisocyanuric acid was carried out in aqueous acetic acid—perchloric
medium. The reactions were found to be first order in case of oxidant and ruthenium(III). Zero order
was observed with the concentrations of sorbitol and mannitol whereas, a positive fractional order was found
in the case of inositol concentration. An inverse fractional order was observed with perchloric acid in oxidation
of three substrates. Arrhenius parameters were calculated and a plausible mechanism was proposed
Shift of Reaction Pathway by Added Chloride Ions in the Oxidation of Aromatic...Ratnakaram Venkata Nadh
Role of added chloride ions on the shift of reaction pathway of oxidation of aromatic ketones (acetophenone,
desoxybenzoin) by dichloroisocyanuric acid (DCICA) was studied in aqueous acetic acid—perchloric
acid medium. Participation of enolic and protonated forms of ketones in the rate determining steps is
manifested from zero and first orders with respect to the oxidant in absence and presence of added chloride
ions, respectively. Positive and negative effects of acid and dielectric constant on the reaction rate were
observed. The observations deduce plausible mechanisms involving (i) rate-determining formation of enol
from the conjugate acid of the ketone (SH+) in the absence of added chloride ions and (ii) rapid formation of
molecular chlorine species from HOCl (hydrolytic species of DCICA) in the presence of added chloride ions,
which then interacts with SH+ in a rate-determining step prior to the rapid steps of product formation. The
order of Arrhenius parameters substantiate the proposed plausible mechanisms based on order of reactants
both in presence and absence of added chloride ions.
Kinetics of Ruthenium(III) Catalyzed and Uncatalyzed Oxidation of Monoethanol...Ratnakaram Venkata Nadh
Kinetics of uncatalyzed and ruthenium(III) catalyzed oxidation of monoethanolamine by N-bromosuccinimide
(NBS) has been studied in an aqueous acetic acid medium in the presence of sodium acetate
and perchloric acid, respectively. In the uncatalyzed oxidation the kinetic orders are: the first order in NBS,
a fractional order in the substrate. The rate of the reaction increased with an increase in the sodium acetate
concentration and decreased with an increase in the perchloric acid concentration. This indicates that free
amine molecules are the reactive species. Addition of halide ions results in a decrease in the kinetic rate,
which is noteworthy. Both in absence and presence of a catalyst, a decrease in the dielectric constant of the
medium decreases the kinetic rate pointing out that these are dipole—dipole reactions. A relatively higher
oxidation state of ruthenium i.e., Ru(V) was found to be the active species in Ru(III) catalyzed reactions. A
suitable mechanism consistent with the observations has been proposed and a rate law has been derived to
explain the kinetic orders.
A novel reversed-phase liquid chromatographic method for the simultaneous det...Ratnakaram Venkata Nadh
In the present study 12 impurities of bisoprolol fumarate (BISO) and hydrochlorothiazide (HCTZ) were
separated simultaneously in a single HPLC method. Out of these 12 impurities, five are potential
degradants, which are validated as per The International Council for Harmonisation of Technical
Requirements for Pharmaceuticals for Human Use (ICH) guidelines. As the two active drug substances
BISO and HCTZ have different solubilities and polarities, the most critical parameters in resolving the
components from each other are pH, temperature, and solvents. The method is precise (RSD < 1.0%),
accurate, linear (r2 > 0.999), robust, and stability indicating in the range of limit of quantification (LOQ)
to 150%. The HPLC method is then migrated to ultra-performance liquid chromatography (UPLC) to
further reduce the run time and solvent consumption, and increase the sample throughput
The emergence of multidrug-resistant TB (MDR-TB) against first-line drugs and extensively drug resistant TB (XDRTB)
due to misuse of second-line anti tubercular drugs (ATDs) is a further concern. Recommended treatment involves
long term and multiple drug therapy with severe side effects. Due to this concern nanoparticle-based systems
have significant potential for treatment and prevention of tuberculosis (TB) to overcome the need to administer
ATDs at high and frequent doses, would assist in improving patient compliance and circumvent hepatotoxic ity
and/or nephrotoxicity/ocular toxicity/ototoxicity associated with the prevalent first-line chemotherapy.
Nanostructured delivery systems constitute a wide range of systems varying from liposomes, micelles, micro- and
nanoemulsions, to polymeric nanoparticles (PNPs ) and solid lipid nanoparticles (SLNs). Pulmonary administration
of inhaled nanoparticles in the form of dry powder inhalers offer particular advantages for pulmonary administration
of anti tubercular drugs (ATDs). Present review comprehensively about different approaches of nanobased
drug delivery, devises and techniques for pulmonary delivery of nanoparticle encapsulated ATD.
Kinetic, isotherm and thermodynamics investigation on adsorption of divalent ...Ratnakaram Venkata Nadh
Three novel and distinct agricultural waste materials, viz., Casuarinas fruit powder (CFP), sorghum stem powder
(SSP) and banana stem powder (BSP) were used as low cost adsorbents for the removal of toxic copper(II) from
aqueous solutions. Acid treated adsorbents were characterized by SEM, EDX and FTIR. Different factors effecting
adsorption capacity were analyzed and the effi ciency order was BSP>SSP>CFP. Based on the extent of compatibility
to Freundlich/Langmuir/D-R/Temkin adsorption isotherm and different models (pseudo-fi rst and second order,
Boyd, Weber’s and Elovich), chemisorption primarily involved in the case of CFP and SSP, whereas, simultaneous
occurrence of chemisorption and physisorption was proposed in the case of BSP. Based on the observations, it was
proposed that three kinetic stages involve in adsorption process viz., diffusion of sorbate to sorbent, intra particle
diffusion and then establishment of equilibrium. These adsorbents have promising role towards removal of Cu(II)
from industrial wastewater to contribute environmental protection.
Kinetic, thermodynamic and equilibrium studies on removal of hexavalent chrom...Ratnakaram Venkata Nadh
Removal of Cr(VI) by biosorption on two agro waste materials, casuarinas fruit powder (CFP) and sorghum
stem powder (SSP), has been investigated. The prepared adsorbent materials were characterized by SEM, EDX,
FTIR and BET. These biomaterials effectively removed Cr(VI) with a maximum removal of 93.35% and 63.75% using
15 gL−1 and 5 gL−1 of CFP and SSP, respectively, at 60 oC with 20mgL−1 initial Cr(VI) concentration in solution. In both
cases of adsorbents, kinetic data of adsorption fitted well in pseudo-second-order in terms of correlation coefficient
(R2). This helps in proposing the process of adsorption as chemical coordination, which is correlated with the thermodynamic
study results conducted at different values of temperature. Langmuir, Freundlich and D-R models were evaluated
for description of metal sorption isotherms. Values of coefficients of intra-particle diffusion and mass transfer have
also been determined at different values of temperature.
Novel coumarin isoxazoline derivatives: Synthesis and study of antibacterial ...Ratnakaram Venkata Nadh
A highly efficient and mild protocol for the syntheses of ethyl-3-
[7-benzyloxy-4-methyl-2-oxo-2H-8-chromenyl]-5-aryl-4,5-dihydro-4-
isoxazole carboxylates and ethyl-3-[7-benzyloxy-3-chloro-4-methyl-2-
oxo-2H-8-chromenyl]-5-aryl-4,5-dihydro-4-isoxazole carboxylates in
good yields via [3 þ 2] cycloaddition of in situ–generated nitrile
oxides from 7-benzyloxy-4-methyl-coumarin hydroxymoylchlorides
and 7-benzyloxy-3-chloro-4-methyl-coumarin hydroxymoylchlorides
respectively with ethyl-3-aryl prop-2-enoate has been developed.
The new compounds are screened for antibacterial activity.
Ultra performance liquid chromatographic method for simultaneous quantificati...Ratnakaram Venkata Nadh
Plerixafor (PLX) injections are administered to patients with cancers of lymphocytes
(non-Hodgkin’s lymphoma) and plasma cells (multiple myeloma). The main
objective of the current study was to develop a short reverse phase chromatographic
method for the simultaneous quantification of PLX and its impurities, in an injection
formulation, to reduce the time required for these quality tests. Furthermore, the
present work describes the role of nonalkyl branched nonquaternary ion pair reagent
in improving the peak shape and reducing column equilibration time. The separation
of PLX and its related substances is pH dependent (optimum pH = 2.50) and was
achieved on an octadecylsilyl (C18) column. The method was validated for its intended
purpose in accordance with the current regulatory guidelines for validation. The
proposed method can be applied for quality control, release, and stability analyses of
active pharmaceutical ingredient, PLX, as well as finished products, PLX injections
Caralluma lasiantha: A review on it’s vital role in Indian Traditional MedicineRatnakaram Venkata Nadh
Caralluma is a genus used as traditional medicine. Caralluma lasiantha is medicinally important due
to existence of pregnane glycosides, which may possess various biological activities. This article thoroughly
reviewed about the usage of C. lasiantha in traditional medicinal system, phytochemicals present in it, profile
identification studies, anti-hyperglycemic effect, antibacterial, antifungal, cytotoxic and antioxidant activities
Phytochemical Investigation of Caralluma lasiantha: Isolation of Stigmasterol...Ratnakaram Venkata Nadh
Stigmasterol, a phytosteroid was isolated for the first time from C. lasiantha using n-hexane as a solvent. Stigmasterol was characterized on the basis of physical, chemical and spectral data (IR, 1H NMR, 13C NMR, 1HNMR, DEPT-45, 90 & 135, and MS) analysis as well as by comparing them to their literature data. A sequence of steps was adopted like saponification, fractional crystallization and gradient elution column chromatography to isolate stigmasterol because some phytosterols possess identical physical properties which makes it difficult to isolate the constituents.
Phytochemical Screening of Caralluma lasiantha Isolation of C21 Pregnane SteroidRatnakaram Venkata Nadh
Phytochemical screening of Caralluma lasiantha was carried out and one C21 pregnane steroid was isolated from chloroform extract. Based on spectroscopic studies (IR, 1H NMR, 13C NMR and ESI-MS) the isolated compound is 3b,14b-dihydroxy-14b-pregn-5-en-20-one which was earlier isolated from other species.
Supercritical fluid (CO2) chromatography for quantitative determination of se...Ratnakaram Venkata Nadh
In the present study, two cancer therapeutic drugs (docetaxel and bortezomib) were separated from their
potential impurities on a chromatographic platform by utilizing CO2 gas (supercritical state) and quantified.
The chromatographic separations were achieved on two short columns BEH-2EP (100mm 3mm, 1.7 mm)
and CHIRALPAK AD-3 (100 mm 4.6 mm, 3 mm) for docetaxel and bortezomib, respectively. The present
work describes the role of organic modifiers in the separation of polar compounds by supercritical fluid
chromatography. The two new methods were fully validated in accordance with the current ICH
(International Council for Harmonization of technical requirements for pharmaceuticals for human use)
guidelines. The stability indicating power of the methods was demonstrated from the stress studies
conducted on the injection formulations of the two compounds. The methods are precise with % RSD of
0.4, linear with the correlation coefficient of r2 $ 0.999 and accurate in the range of 50–150% of the
target assay concentration. The two methods can be equally employed for the assay determination of
docetaxel and bortezomib APIs as well.
A convenient new and efficient commercial synthetic route for dasatinib (Spry...Ratnakaram Venkata Nadh
A new and efficient synthetic route for dual-Src/Abl kinase inhibitor
dasatinib (Sprycel®), an anticancer drug, is described. This commercially
viable process yields dasatinib monohydrate free of potential impurities
with consistent yield of 68% in route A and 61% in route B with HPLC
purity >99.80% over four stages.
Utilization of agro-waste for removal of toxic hexavalent chromium: surface i...Ratnakaram Venkata Nadh
Abundantly available agricultural waste materials
(banana bunch, sorghum stem and casuarinas fruit) are
processed with negligible cost and are found to be highly
suitable as biosorbents for chromium(VI) removal from
aqueous environment due to high surface area and functional
groups of adsorbents. The equilibrium data have
been analyzed for the adsorbate–adsorbate/adsorbent
interactions and found to be fitted to the data in the order,
Hill–de Boer C Fowler–Guggenheim % Frumkin[Kiselev.
To determine the characteristic parameters for process
design, mass transfer studies have been carried out using
two-parameter isotherm models (Harkins–Jura, Halsey,
Smith, El-Awady and Flory–Huggins) and three-parameter
isotherm models (Redlich–Peterson and Sips) which are
applied to the experimental data. The fitness of the isotherms
describes that both mono- and multilayer adsorptions
occur in the present studied three biosorbents in
preference to the latter. The mechanism of adsorption has
been studied using diffusion kinetic models (viz. liquid film
diffusion, Dunwald–Wagner intra-particle diffusion model
and moving boundary model) and described the possibility
of diffusion in the order of banana bunch–stem powder[
sorghum stem powder[casuarinas fruit powder in
terms of diffusion coefficients. In essence of all the results,
the selected adsorbents can be used as a potential adsorbent
for the removal of Cr(VI) from aqueous solutions.
Evaluation of in vitro antibacterial activity of Caralluma lasiantha for scie...Ratnakaram Venkata Nadh
Caralluma lasiantha is used as a traditional medicine in India to heal body
heat and inflammations. In order to find out a scientific validation for the Indian
traditional knowledge, antibacterial activity of C. lasiantha extracts was studied
against inflammation causing bacteria (viz., Staphylococcus aureus, Escherichia coli,
Streptococcus Sp., Bacillus subtilis, Enterobacter aerogenes, Klebsiella pneumoniae)
along with other Gram-positive and Gram-negative bacteria. Solvents with different
polarity were used for extraction from dry roots and stems. Minimum inhibitory
concentrations (MIC) were also studied. Differential antibacterial activity was
exhibited by extracts and higher inhibition potential against Gram-positive bacteria
was explained. The observed antibacterial activities were correlated with the chemical
structures of phytochemicals present in C. lasiantha. Anti-inflammation activities
are related to C. lasiantha extracts through their antibacterial activities.
Novel Hybrid Molecules of Isoxazole Chalcone Derivatives: Synthesis and Study...Ratnakaram Venkata Nadh
medicine due to their significant role in the treatment of different health problems.
Methods: We have synthesized new series of isoxazole-chalcone conjugates (14a-m) by the
Claisen-Schmidt condensation of suitable substituted acetophenones with isoxazole aldehydes (12a-d).
In vitro cytotoxic activity of the synthesized compounds was studied against four different selected
human cancer cell lines by using sulforhodamine B (SRB) method.
Results: The adopted scheme resulted in good yields of new series of isoxazole-chalcone
conjugates (14a-m). Potent cytotoxic activity was observed for compounds -14a, 14b, 14e, 14i, 14j
and 14k against prostate DU-145 cancer cell line.
Conclusion: The observed potent cytotoxic activities were due to the presence of 3,4,5-
trimethoxyphenyl group.
New Directions in Targeted Therapeutic Approaches for Older Adults With Mantl...i3 Health
i3 Health is pleased to make the speaker slides from this activity available for use as a non-accredited self-study or teaching resource.
This slide deck presented by Dr. Kami Maddocks, Professor-Clinical in the Division of Hematology and
Associate Division Director for Ambulatory Operations
The Ohio State University Comprehensive Cancer Center, will provide insight into new directions in targeted therapeutic approaches for older adults with mantle cell lymphoma.
STATEMENT OF NEED
Mantle cell lymphoma (MCL) is a rare, aggressive B-cell non-Hodgkin lymphoma (NHL) accounting for 5% to 7% of all lymphomas. Its prognosis ranges from indolent disease that does not require treatment for years to very aggressive disease, which is associated with poor survival (Silkenstedt et al, 2021). Typically, MCL is diagnosed at advanced stage and in older patients who cannot tolerate intensive therapy (NCCN, 2022). Although recent advances have slightly increased remission rates, recurrence and relapse remain very common, leading to a median overall survival between 3 and 6 years (LLS, 2021). Though there are several effective options, progress is still needed towards establishing an accepted frontline approach for MCL (Castellino et al, 2022). Treatment selection and management of MCL are complicated by the heterogeneity of prognosis, advanced age and comorbidities of patients, and lack of an established standard approach for treatment, making it vital that clinicians be familiar with the latest research and advances in this area. In this activity chaired by Michael Wang, MD, Professor in the Department of Lymphoma & Myeloma at MD Anderson Cancer Center, expert faculty will discuss prognostic factors informing treatment, the promising results of recent trials in new therapeutic approaches, and the implications of treatment resistance in therapeutic selection for MCL.
Target Audience
Hematology/oncology fellows, attending faculty, and other health care professionals involved in the treatment of patients with mantle cell lymphoma (MCL).
Learning Objectives
1.) Identify clinical and biological prognostic factors that can guide treatment decision making for older adults with MCL
2.) Evaluate emerging data on targeted therapeutic approaches for treatment-naive and relapsed/refractory MCL and their applicability to older adults
3.) Assess mechanisms of resistance to targeted therapies for MCL and their implications for treatment selection
Lung Cancer: Artificial Intelligence, Synergetics, Complex System Analysis, S...Oleg Kshivets
RESULTS: Overall life span (LS) was 2252.1±1742.5 days and cumulative 5-year survival (5YS) reached 73.2%, 10 years – 64.8%, 20 years – 42.5%. 513 LCP lived more than 5 years (LS=3124.6±1525.6 days), 148 LCP – more than 10 years (LS=5054.4±1504.1 days).199 LCP died because of LC (LS=562.7±374.5 days). 5YS of LCP after bi/lobectomies was significantly superior in comparison with LCP after pneumonectomies (78.1% vs.63.7%, P=0.00001 by log-rank test). AT significantly improved 5YS (66.3% vs. 34.8%) (P=0.00000 by log-rank test) only for LCP with N1-2. Cox modeling displayed that 5YS of LCP significantly depended on: phase transition (PT) early-invasive LC in terms of synergetics, PT N0—N12, cell ratio factors (ratio between cancer cells- CC and blood cells subpopulations), G1-3, histology, glucose, AT, blood cell circuit, prothrombin index, heparin tolerance, recalcification time (P=0.000-0.038). Neural networks, genetic algorithm selection and bootstrap simulation revealed relationships between 5YS and PT early-invasive LC (rank=1), PT N0—N12 (rank=2), thrombocytes/CC (3), erythrocytes/CC (4), eosinophils/CC (5), healthy cells/CC (6), lymphocytes/CC (7), segmented neutrophils/CC (8), stick neutrophils/CC (9), monocytes/CC (10); leucocytes/CC (11). Correct prediction of 5YS was 100% by neural networks computing (area under ROC curve=1.0; error=0.0).
CONCLUSIONS: 5YS of LCP after radical procedures significantly depended on: 1) PT early-invasive cancer; 2) PT N0--N12; 3) cell ratio factors; 4) blood cell circuit; 5) biochemical factors; 6) hemostasis system; 7) AT; 8) LC characteristics; 9) LC cell dynamics; 10) surgery type: lobectomy/pneumonectomy; 11) anthropometric data. Optimal diagnosis and treatment strategies for LC are: 1) screening and early detection of LC; 2) availability of experienced thoracic surgeons because of complexity of radical procedures; 3) aggressive en block surgery and adequate lymph node dissection for completeness; 4) precise prediction; 5) adjuvant chemoimmunoradiotherapy for LCP with unfavorable prognosis.
These simplified slides by Dr. Sidra Arshad present an overview of the non-respiratory functions of the respiratory tract.
Learning objectives:
1. Enlist the non-respiratory functions of the respiratory tract
2. Briefly explain how these functions are carried out
3. Discuss the significance of dead space
4. Differentiate between minute ventilation and alveolar ventilation
5. Describe the cough and sneeze reflexes
Study Resources:
1. Chapter 39, Guyton and Hall Textbook of Medical Physiology, 14th edition
2. Chapter 34, Ganong’s Review of Medical Physiology, 26th edition
3. Chapter 17, Human Physiology by Lauralee Sherwood, 9th edition
4. Non-respiratory functions of the lungs https://academic.oup.com/bjaed/article/13/3/98/278874
Flu Vaccine Alert in Bangalore Karnatakaaddon Scans
As flu season approaches, health officials in Bangalore, Karnataka, are urging residents to get their flu vaccinations. The seasonal flu, while common, can lead to severe health complications, particularly for vulnerable populations such as young children, the elderly, and those with underlying health conditions.
Dr. Vidisha Kumari, a leading epidemiologist in Bangalore, emphasizes the importance of getting vaccinated. "The flu vaccine is our best defense against the influenza virus. It not only protects individuals but also helps prevent the spread of the virus in our communities," he says.
This year, the flu season is expected to coincide with a potential increase in other respiratory illnesses. The Karnataka Health Department has launched an awareness campaign highlighting the significance of flu vaccinations. They have set up multiple vaccination centers across Bangalore, making it convenient for residents to receive their shots.
To encourage widespread vaccination, the government is also collaborating with local schools, workplaces, and community centers to facilitate vaccination drives. Special attention is being given to ensuring that the vaccine is accessible to all, including marginalized communities who may have limited access to healthcare.
Residents are reminded that the flu vaccine is safe and effective. Common side effects are mild and may include soreness at the injection site, mild fever, or muscle aches. These side effects are generally short-lived and far less severe than the flu itself.
Healthcare providers are also stressing the importance of continuing COVID-19 precautions. Wearing masks, practicing good hand hygiene, and maintaining social distancing are still crucial, especially in crowded places.
Protect yourself and your loved ones by getting vaccinated. Together, we can help keep Bangalore healthy and safe this flu season. For more information on vaccination centers and schedules, residents can visit the Karnataka Health Department’s official website or follow their social media pages.
Stay informed, stay safe, and get your flu shot today!
MANAGEMENT OF ATRIOVENTRICULAR CONDUCTION BLOCK.pdfJim Jacob Roy
Cardiac conduction defects can occur due to various causes.
Atrioventricular conduction blocks ( AV blocks ) are classified into 3 types.
This document describes the acute management of AV block.
TEST BANK for Operations Management, 14th Edition by William J. Stevenson, Ve...kevinkariuki227
TEST BANK for Operations Management, 14th Edition by William J. Stevenson, Verified Chapters 1 - 19, Complete Newest Version.pdf
TEST BANK for Operations Management, 14th Edition by William J. Stevenson, Verified Chapters 1 - 19, Complete Newest Version.pdf
Title: Sense of Taste
Presenter: Dr. Faiza, Assistant Professor of Physiology
Qualifications:
MBBS (Best Graduate, AIMC Lahore)
FCPS Physiology
ICMT, CHPE, DHPE (STMU)
MPH (GC University, Faisalabad)
MBA (Virtual University of Pakistan)
Learning Objectives:
Describe the structure and function of taste buds.
Describe the relationship between the taste threshold and taste index of common substances.
Explain the chemical basis and signal transduction of taste perception for each type of primary taste sensation.
Recognize different abnormalities of taste perception and their causes.
Key Topics:
Significance of Taste Sensation:
Differentiation between pleasant and harmful food
Influence on behavior
Selection of food based on metabolic needs
Receptors of Taste:
Taste buds on the tongue
Influence of sense of smell, texture of food, and pain stimulation (e.g., by pepper)
Primary and Secondary Taste Sensations:
Primary taste sensations: Sweet, Sour, Salty, Bitter, Umami
Chemical basis and signal transduction mechanisms for each taste
Taste Threshold and Index:
Taste threshold values for Sweet (sucrose), Salty (NaCl), Sour (HCl), and Bitter (Quinine)
Taste index relationship: Inversely proportional to taste threshold
Taste Blindness:
Inability to taste certain substances, particularly thiourea compounds
Example: Phenylthiocarbamide
Structure and Function of Taste Buds:
Composition: Epithelial cells, Sustentacular/Supporting cells, Taste cells, Basal cells
Features: Taste pores, Taste hairs/microvilli, and Taste nerve fibers
Location of Taste Buds:
Found in papillae of the tongue (Fungiform, Circumvallate, Foliate)
Also present on the palate, tonsillar pillars, epiglottis, and proximal esophagus
Mechanism of Taste Stimulation:
Interaction of taste substances with receptors on microvilli
Signal transduction pathways for Umami, Sweet, Bitter, Sour, and Salty tastes
Taste Sensitivity and Adaptation:
Decrease in sensitivity with age
Rapid adaptation of taste sensation
Role of Saliva in Taste:
Dissolution of tastants to reach receptors
Washing away the stimulus
Taste Preferences and Aversions:
Mechanisms behind taste preference and aversion
Influence of receptors and neural pathways
Impact of Sensory Nerve Damage:
Degeneration of taste buds if the sensory nerve fiber is cut
Abnormalities of Taste Detection:
Conditions: Ageusia, Hypogeusia, Dysgeusia (parageusia)
Causes: Nerve damage, neurological disorders, infections, poor oral hygiene, adverse drug effects, deficiencies, aging, tobacco use, altered neurotransmitter levels
Neurotransmitters and Taste Threshold:
Effects of serotonin (5-HT) and norepinephrine (NE) on taste sensitivity
Supertasters:
25% of the population with heightened sensitivity to taste, especially bitterness
Increased number of fungiform papillae
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Determination of Satranidazole through Ion-Associative Complex Reaction
1. Asian Pub. Corp.
www.asianpubs.org
Asian Journal of Organic
& Medicinal Chemistry
Volume: 4 Year: 2019
Issue: 1 Month: January–March
pp: 23–27
DOI: https://doi.org/10.14233/ajomc.2019.AJOMC-P166
Received: 3 December 2018
Accepted: 19 February 2019
Published: 30 March 2019
Author affiliations:
1
Department of Chemistry, K.B.N. College,Vijayawada-520001, India
2
DepartmentofChemistry, GITAM University-Bengaluru, Bengaluru-
562163, India
3
Department of Chemistry,Acharya Nagarjuna University, Nagarjuna
Nagar-522510, India
To whom correspondence to be addressed:
E-mail: katarekirankumar@gmail.com
Determination of Satranidazole through
Ion-Associative Complex Reaction
K. Kiran Kumar1,
, R.Venkata Nadh2
,
M. Siva Kishore1
and G. Giri Prasad3
K E Y W O R D S
Satranidazole, Ion-Associative complex,Tropaeolin OOO,Validation,
Visible spectrophotometry.
ARTICLE
Available online at: http://ajomc.asianpubs.org
I N T R O D U C T I O N
Satranidazole {1-methylsulfonyl-3-(1-methyl-5-nitro-2-
imidazolyl)-2-imidazolidinone} (Fig. 1) is a nitroimidazole
derivative and widely used as antiprotozoal agent in the treat-
ment of amoebiasis [1]. Literature survey revealed that few
analytical methods have been developed for the determination
of satranidazole in pharmaceutical formulations and biological
materials include spectrophotometric [2-5], HPLC [6-11],
HPTLC [12,13] and electron-capture gas chromatographic
determination [14].
NN
S
O
O
O
N
N
O2N
Fig. 1. Structure of satranidazole
Previously reported spectrophotometric methods [2,4] for
the determination of satranidazole in pharmaceutical formu-
lationsandbiologicalmaterialswerecomplicatedandnotecono-
mical. The aim of the present study is to develop a relatively
simple, sensitive, validated and low-cost visible spectropho-
tometric method for the determination of satranidazole in bulk
drug and pharmaceutical dosage form.
A simple, selective, accurate and low-cost spectrophotometric method
has been described for determination of satranidazole in bulk and
pharmaceutical formulations. The developed method involves the
formation of chloroform extractable colored ion-association complex
of satranidazole with Tropaeolin OOO (TPooo). The extracted colored
complex showed absorbance maximum at wavelength 484 nm and
obeying Beer′s law in the concentration 4-20 µg mL-1
with the
correlation coeffiecent of 0.9998. The results of statistical analysis of
the proposed method reveals high accuracy and good precession.Thus,
the proposed method can be used commercially for the determination
of satranidazole in bulk and pharmaceutical formulations.
A B S T R A C T
2. In quality control laboratories of the developing countries,
the mostly adopted quantitative method for determination of
pharmaceutical drugs is visible spectrophotometry.Among the
different reactions engaged in visible spectrophotometric
estimation of pharmaceutical drugs, ion association complex
[15-20] formation and oxidation [21,22] methods are found
to be acceptable and sensitive methods. In addition, the former
is very easy to accomplish. Out of all the existing various tech-
niques, formation of coloured ion association complex is a
prevalent methodology for the determination of pharmaceutical
drugs in a quantitative manner. Ion association complex forma-
tion method can be easily extended for all such pharmaceutical
drugs holding at least one hetero atom (like nitrogen or oxygen)
having lone pair of electrons. So, such compounds are proto-
nated due to acceptance of proton(s) and yield cations. Acidic
dyes undergo hydrolysis in aqueous medium to form anions
and are capable to promote the generation of an ion association
complex with the cationic form of the drug [18].
Tropaeolin OOO (TPooo) is an azo dye and its chemical
name is 4-(4-hydroxy-1-naphthylazo)benzenesulfonic acid
sodium salt. Other names of it are Orange I, α-naphthol orange
and acid orange 20. The sodium sulfonate group of TPooo
experiences ionization in acidic medium to result in a negat-
ively charged anion. The so formed ion association complex
is extractable in organic solvent and absorbance of organic
phase can be measured spectrophotometrically [17].The added
gain of ion association complex is its application for precise
determination of target compound in spite of theAPI′s existence
with various formulation constituents. Driven by the advantages
mentioned above, the present proposed study enlightens to
establish a process, that is grounded on formation of a soluble
ion-pair complex with the dissociated form of an acidic chromo-
genic dye like Tropaeolin OOO.
E X P E R I M E N T A L
An Elico, UV-visible digital spectrophotometer [SL-159]
with 1 cm matched quartz cells was used for the spectral and
absorbance measurements. For pH measurements, an Elico
LI-120 digital pH meter was used. All the reagents used in this
assay were of analytical grade and the reagent solutions were
prepared using double distilled water.
Preparation of standard drug solutions: The pharma-
ceutical grade pure sample of satranidazole (99.56 %) was
procured from Celon Laboratories Limited, India. The stock
solution (1.0 mg mL-1
) of satranidazole was prepared by disso-
lving 100 mg of drug in 10 mL of methanol and made up to
100 mL with distilled water to get a clear solution.Appropriate
volumes of this stock solution were diluted step wise to get
the working standard solutions with concentrations of 80 µg/
mL for method.
Preparation of tablets solution: About 10 tablets of
SATROGYL (300 mg) were pulverized to fine powder and the
powder equivalent to 100 mg of satranidazole was accurately
weighed and transferred into a 100 mL calibrated flask, 60
mL of methanol was added and the contents shaken thoroughly
for 15-20 min to extract the drug into the liquid phase. The
volume was finally diluted to the mark with water, mixed well
and filtered throughWhatmann filter paper No. 41. The filtrate
was made up to mark with distilled water in a 100 mL volu-
metric flask. A suitable volume of this filtrate was accurately
diluted with water and this solution was used for the determi-
nation of satranidazole as per the recommended procedures.
Preparation of reagents
TPooo (0.1 % w/v): Aqueous solution of TPooo dye
solution was prepared by dissolving 100 mg dye in 100 mL of
double distilled water.
0.1 N HCl: Prepared by dissolving 8.6 mL of HCl in 100
mL of double distilled water.
Recommended procedures:Aliquots of standard satrani-
dazole (80 µg mL-1
) solution ranging from 0.5-2.5 mL were
transferred into a series of 125 mL separating funnels. To that
2 mL of TPooo (0.1 %) and 1.0 mL of 0.1 N HCl were added
and the total volume of aqueous phase was made up to 10 mL
with distilled water.To each funnel, about 10 mL of chloroform
was added and the contents were shaken for 2 min. Later, the
two phases were allowed to separate and the absorbance of
chloroform layer was measured at 484 nm against the corresp-
onding reagent blank. The amount of satranidazole present in
the sample solution was computed from its calibration curve
(Fig. 2).
0.20
0.18
0.16
0.14
0.12
0.10
0.08
0.06
0.04
0.02
Absorbance
444 452 460 468 476 484 492 500 508 516
Wavelength (nm)
Tpooo = 0.1 % W/V
Fig. 2. Absorption spectra of satranidazole
R E S U L T S A N D D I S C U S S I O N
Optimization of experimental conditions:The optimum
conditions were fixed based on the study of effects of various
parameters viz., type of acid, conc. of acid, conc. of dye (TPooo),
shaking time, temperature, choice of organic solvent, ratio of
organic phase to aqueous phase, intensity and stability of the
coloured species in organic phase. Controlled impediments were
performed by varying one and fixing the other parameters.
Then absorbance was measured at λmax (484 nm) for a series
of solutions and the results are incorporated in Table-1.
Optical characteristics:The proposed method is validated
as per the existing ICH guidelines [23,24]. The Beer′s law and
24 Kumar et al.
3. Ringbom plots of the proposed methods were recorded
graphically (Figs. 3 and 4). Regression analysis of the Beer′s
law data using the method of least squares was made to evaluate
the slope (b), intercept (a) and correlation coefficient (r2
) for this
method and the values are presented in Table-2. The values of
optical characteristics (Beer′s law limits, molar absorptivity
and Sandell’s sensitivity) for method are also given in Table-2.
0.40
0.35
0.30
0.25
0.20
0.15
0.10
0.05
0
Absorbance
0 5 10 15 20 25 30
Concentration (µg/mL)
y = 0.0150x + 0.0016
R = 0.9994
2
Fig. 3. Beer’s law plot of satranidazole
30
40
50
60
70
80
90
100
Transmittance(%)
0.5 0.8 1.1 1.4 1.7
log concentration
Fig. 4. Ringbom plot of satranidazole
TABLE-2
RESULTS OF OPTICAL, REGRESSION, PRECISION
AND ACCURACY OF THE PROPOSED METHOD
Parameter Tpooo
λmax (nm) 484
Beer’s law limits (µg/mL) 4.0-20.0
Molar absorptivity (1 mol–1
cm–1
) 6.946 × 103
Sandell’s sensitivity (µg cm-2
/0.001 absorbance unit) 0.12455
Optimum photometric range (µg/mL) 6.0 -18.0
Regression equation (Y = a + bc); slope (b) 0.0219
Intercept (a) 0.0066
Correlation coefficient (r) 0.9998
Standard deviation on intercept (Sa) 1.2792 × 10-4
Standard deviation on slope (Sb) 2.2174 × 10-4
Standard error on estimation (Se) 2.8048 × 10-3
LOD (µg/mL) 0.0173
LOQ (µg/mL) 0.0579
Relative standard deviation (%)* 1.278
% Range of error (confidence limits)
0.05 level 1.069
0.01 level 1.581
*Average of six determinations considered
Precision:Theprecisionoftheproposedmethodwasascer-
tained from the absorbance values obtained by actual deter-
mination of six replicates of a fixed amount of satranidazole.
The % RSD (percent relative standard deviation) and percent
range of error (at 0.05 and 0.01 confidence limits) was calcul-
ated for the proposed method (Table-2).
Accuracy:Theaccuracywasevaluatedaspercentagerelative
error between the measured concentrations and taken concen-
trations for satranidazole. The results obtained are compiled
in Table-2.
Analysis of pharmaceutical formulations: The proposed
method was applied to determine satranidazole in commercial
brand (Satrogyl, 300 mg). The results were compared with
those of the literature method. Statistical analysis of the results
using Student's t-test for accuracy and F-test for precision
revealednosignificantdifferencebetweentheproposedmethods
and the literature method at the 95 % confidence level with
respect to accuracy and precision. The results of the proposed
methods are summarized in Table-3.
Chemistry of the colored species: Satranidazole consists
of different analytically useful functional groups such as nitro
group in the imidazole system and tertiary nitrogen group of
TABLE-1
OPTIMUM CONDITIONS ESTABLISHED IN METHOD-TPoooFOR SATRANIDAZOLE
Parameter Optimum range
Conditions in
procedure
Remarks
λmax (nm) 480-490 484 –
Effect of volume of dye TPooo 0.5-3.0 mL 2.0 mL 2.0 mL of TPooo of dye was necessary for covering the broad range
of Beer’s law limits.
Choice of organic solvent for
extraction of colored complex
Chloroform Chloroform CHCl3 was preferred for its selective extraction of the colored drug-
dye complex from the aqueous phase.
Effect of shaking time (min) 1-5 min 2 min Constant absorbance values were obtained for the shaking period of
1-5 min.
Effect of temperature (°C) on the
colored species
Laboratory
temperature
(28 ± 5)
Laboratory
temperature
(28 ± 5)
At low temperature (< 20 °C) and at high temperature (>35 °C) the
extraction of the colored species was found to be improper and the
stability of the colored species was found to be very less.
Stability of the colored species – 60 min The colored species after separation from organic phase was stable
for 60 min, after wards the absorbance gradually decreases.
Asian Journal of Organic & Medicinal Chemistry 25
4. N
N
CH3
O2
N
NN
SO2
O
N
N
CH3
O2
N
NN
SO2
OH
N
N
CH3
O2N
NN
SO2
OH
NaO3S N N OH O3S N N OH
O3
S N N OH
N
N
CH3
O2N
NN
SO2
OH
O3S N N OH
-
HCl
-
-
Cationic form of Stranidazole
Anionic form of TPooo
+
+
+
Cationic form of Stranidazole
Anionic form of TPooo
TPooo
+
Ion pair complex
Fig. 5. Reaction of satranidazole with TPooo
TABLE-3
ASSAY AND RECOVERY OF SATRANIDAZOLE IN DOSAGE FORM
Proposed method
Pharmaceutical
formulation
Labeled amount
(mg) Amount found
mean* ± S.D (mg)
T value F value
Found by reference
method** ± S.D (mg)
% Recovery by
proposed method
Satrogyl 300.00 299.95 ± 0.79 0.33 1.300 299.99 ± 0.204 99.96 ± 0.18
*Average ± standard deviation of six determinants the t and F- values refer to comparison of the proposed method.
Theoretical values at 95 % confidence limits t = 2.571 and F = 5.05.
*Average of six determinations. **Reference Method – [Ref. 2]
varied reactivity and it is difficult to say the exact nature of
the existing coloured species of reasonable stability in each
one of the proposed method formed with the chromogenic
reagents. Reaction involved is ion pair association complex
with the positive charge of the basic drug (protonated amino
group in satranidazole) with the negative charge of acidic dye
TPooo. The chemistry of coloured species formed in proposed
methodfortheassayofsatranidazolehasbeenpresentedinFig. 5.
Conclusion
A new visible spectrophotometric method for determi-
nation of satranidazole has been developed using chromogenic
dye reagent Tropaeolin OOO (TPooo). The method was found
to be simple, cost effective, sensitive and reproducible. From
the analytical data reported, the LOD and LOQ values reported
by the proposed method indicating high sensitivity of the
proposed method. The simplicity, selectivity and robustness
achieved by the proposed methods advocate their applicability
in routine quality control of satranidazole tablets.
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Asian Journal of Organic & Medicinal Chemistry 27