Ion pair chromatography for pharmacy studentsabhishek rai
Ion-Pair Chromatography
A GENERALISED OVERVIEW
Chromatography
HPLC
Reverse Phase Chromatography
Ion Pair Chromatography
Ion Pair Reagent
Mechanism of Ion Pair Chromatography
Ion Pair Wash Procedure
The dissolution test is an important means of assuring the continuing performance of non-solution orally administered drug products. The development of a dissolution test procedure is briefly discussed in USP general information chapter In Vitro and In Vivo Evaluation of Dosage Forms 1088, whereas general information chapter Validation of Compendial Procedures 1225 gives limited validation information for dissolution testing. Neither of these two chapters provides a level of detail and focus sufficient for dissolution testing. In 2001, a Stimuli article provided an initial rationale and discussion of content for a new general information chapter. The new chapter, The Dissolution Procedure: Development and Validation 1092, was intended to supplement the information in 1088 and 1225 and provided step-by-step detail for development and validation as well as offering information on new technology and equipment. In 2006, the chapter became official with the Second Supplement to USP 29–NF 24 (2–4).
The General Chapters—Dosage Forms Expert Committee 2010–2015 placed the review and possible revision of The Dissolution Procedure: Development and Validation 1092 on its work plan for the 2010–2015 revision cycle (2011) .
Drug Regulations has prepared this presentation based on the proposed chapter.
Ion pair chromatography for pharmacy studentsabhishek rai
Ion-Pair Chromatography
A GENERALISED OVERVIEW
Chromatography
HPLC
Reverse Phase Chromatography
Ion Pair Chromatography
Ion Pair Reagent
Mechanism of Ion Pair Chromatography
Ion Pair Wash Procedure
The dissolution test is an important means of assuring the continuing performance of non-solution orally administered drug products. The development of a dissolution test procedure is briefly discussed in USP general information chapter In Vitro and In Vivo Evaluation of Dosage Forms 1088, whereas general information chapter Validation of Compendial Procedures 1225 gives limited validation information for dissolution testing. Neither of these two chapters provides a level of detail and focus sufficient for dissolution testing. In 2001, a Stimuli article provided an initial rationale and discussion of content for a new general information chapter. The new chapter, The Dissolution Procedure: Development and Validation 1092, was intended to supplement the information in 1088 and 1225 and provided step-by-step detail for development and validation as well as offering information on new technology and equipment. In 2006, the chapter became official with the Second Supplement to USP 29–NF 24 (2–4).
The General Chapters—Dosage Forms Expert Committee 2010–2015 placed the review and possible revision of The Dissolution Procedure: Development and Validation 1092 on its work plan for the 2010–2015 revision cycle (2011) .
Drug Regulations has prepared this presentation based on the proposed chapter.
The drug or drug combination may not be official in any pharmacopoeias.
A proper analytical procedure for the drug may not be available in the literature due to patent regulations.
Analytical methods may not be available for the drug in the form of a formulation due to the interference caused by the formulation excipients.
Analytical methods for the quantitation of the drug in biological fluids may not be available.
Analytical methods for a drug in combination with other drugs may not be available.
The existing analytical procedures may require expensive reagents and solvents. It may also involve cumbersome extraction and separation procedures and these may not be reliable.
To recommend acceptable amounts for residual solvents in pharmaceuticals for the safety of the patient. The guideline recommends use of less toxic solvents and describes levels considered to be toxicologically acceptable for some residual solvents.
The guideline applies to all dosage forms and routes of administration.
This guidelines does not address all possible solvents, only those identified in drugs at that time, neither address solvents intentionally used as excipients nor solvates.
The maximum acceptable intake per day of residual solvent in pharmaceutical products is defined as “permitted daily exposure” (PDE)
Previously, another terms were used like “Tolerable daily intake” (TDI) & “Acceptable daily intake” (ADI) by different organization & authorities, but now usually this new term “PDE” is used
This poster describes analytical operating conditions for analysis of US EPA Method 8260C1, Revision 3, August 2006, and includes BFB tune parameters, calibration details, and a complete MDL and Precision and Accuracy study for almost 100 target compounds at multiple concentrations.
Development and validation of GC-MS method for analysis of chloropyramine hyd...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).
The drug or drug combination may not be official in any pharmacopoeias.
A proper analytical procedure for the drug may not be available in the literature due to patent regulations.
Analytical methods may not be available for the drug in the form of a formulation due to the interference caused by the formulation excipients.
Analytical methods for the quantitation of the drug in biological fluids may not be available.
Analytical methods for a drug in combination with other drugs may not be available.
The existing analytical procedures may require expensive reagents and solvents. It may also involve cumbersome extraction and separation procedures and these may not be reliable.
To recommend acceptable amounts for residual solvents in pharmaceuticals for the safety of the patient. The guideline recommends use of less toxic solvents and describes levels considered to be toxicologically acceptable for some residual solvents.
The guideline applies to all dosage forms and routes of administration.
This guidelines does not address all possible solvents, only those identified in drugs at that time, neither address solvents intentionally used as excipients nor solvates.
The maximum acceptable intake per day of residual solvent in pharmaceutical products is defined as “permitted daily exposure” (PDE)
Previously, another terms were used like “Tolerable daily intake” (TDI) & “Acceptable daily intake” (ADI) by different organization & authorities, but now usually this new term “PDE” is used
This poster describes analytical operating conditions for analysis of US EPA Method 8260C1, Revision 3, August 2006, and includes BFB tune parameters, calibration details, and a complete MDL and Precision and Accuracy study for almost 100 target compounds at multiple concentrations.
Development and validation of GC-MS method for analysis of chloropyramine hyd...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).
This poster describes a GCMS purge-and-trap (P&T) method validation study conducted to evaluate operating conditions for the existing US EPA Method 624 VOC list, using updated technology and advanced GCMS instrumentation.
For more information, go to www.ssi.shimadzu.com and follow Shimadzu on Twitter at @ShimadzuSSI. Thanks for viewing.
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.
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.
Stability indicating analytical method development and validation for estimat...SriramNagarajan18
Stability indicating analytical method development and validation for estimation of Ceftazidime and Avibactam in bulk and pharmaceutical dosage form using RP-HPLC
Method Development and Validation for Estimation of Oral Hypoglycaemic Drug D...ijtsrd
HPLC is a chromatographic technique employed in active compound chemistry and biochemistry to separate a mixture and substances with the goal of identifying, measuring, and purifying the different components of the mixture. Its a much better variety of column and traditional chromatography. The objective of the research work is to develop and validate a simple and accurate reverse phase chromatographic method to estimate amount of drug in dosage form. The developed method successfully can be applied to estimate the amount of Dapagliflozin in tablet dosage form. After oral administration of dapagliflozin, the maximum plasma concentration Concentration max under two hours. High performance liquid chromatographic system was alleviated according to the chromatographic settings. After attaining the steady base line, to verify the system suitability, a single 40 µg ml of standard solution proportional to 100 test concentration of dapagliflozin was injected into the HPLC system. The gradient mobile phase flow rate programming assisted in optimising the lengthy run duration and resolution of sample analysis, making the approach more cost effective and quick. Validation of the developed and optimized HPLC method was carried out according to ICH guidelines with respect to parameters such as linearity, specificity, precision and accuracy. Junaid Ahmed | Himanchal Sharma | Shiva Teotia "Method Development and Validation for Estimation of Oral Hypoglycaemic Drug Dapagliflozinina Tablet Dosage form by the Employment of Rp-HPLC" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-5 | Issue-6 , October 2021, URL: https://www.ijtsrd.com/papers/ijtsrd46395.pdf Paper URL : https://www.ijtsrd.com/pharmacy/analytical-chemistry/46395/method-development-and-validation-for-estimation-of-oral-hypoglycaemic-drug-dapagliflozinina-tablet-dosage-form-by-the-employment-of-rphplc/junaid-ahmed
Development and Validation of Reversed Phase-High-Performance Liquid Chromato...BRNSS Publication Hub
A simple, accurate, precise, and robust in vitro methods developed and validated for measurement of drug release in Aminocaproic Acid tablets. High-performance liquid chromatography (HPLC) method for quantification of drug in dissolution samples of Aminocaproic Acid tablet is developed and validated. 0.1 N Hydrochloric acid is used as dissolution medium and Basket (USP-I) as apparatus at 100 rpm. The sample was withdrawn after 60 min. The developed HPLC method was used for quantitative estimation of drug release in dissolution samples of Aminocaproic Acid tablet. Chromatogram was run through Inertsil ODS 3V, (250 × 4.6 mm), 5 μm. Mobile phase containing buffer solution and methanol in the pumped through column at a flow rate of 1 ml/min. Buffer used in this method was 13.3 g sodium dihydrogen phosphate monohydrate, 500 mg of Heptane-1-sulfonic acid sodium salt, and 1.0 mL of Triethylamine buffer with pH 2.20 adjusted by orthophosphoric acid. Optimized wavelength for Aminocaproic acid was 210 nm. Retention time of Aminocaproic acid was found about 4.0 min; linearity range was 132.605 μg/ml–828.787 μg/ml. The new method was evaluated according to ICH guideline and as far as validation results are concern correlation coefficient value was 0.9999 for the very compound, percentage recovery 100.0%, repeatability results relative standard deviation 0.9 for Aminocaproic acid. The developed HPLC method was found to be a simple and rapid one for regular analysis in professional laboratory.
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
A Simple Rp- HPLC Method for Simultaneous Estimation of Six Cardiovascular Dr...iosrjce
A simple, convenient Rp-HPLC method has been developed and validated for the simultaneous
estimation of Metolazone, Indapamide, Nebivolol, Rosuvastatin, Olmesartan and Spironolactone. The column
used was an Inertsil ODS 3 V column of 250 mm length × 4.6 mm ID, with 3 micron particle size of adsorbent.
Separation was achieved using isocratic elution in a buffer-acetonitrile-methanol mobile phase at a flow rate of
1.2 ml/min. The detection was performed at wavelength of 225 nm using a UV detector. The column temperature
was 450C and injection volume was 20µl. The method was validated for precision, linearity and accuracy. The
% RSD for all the drugs was found to be less than 2 %. The correlation coefficient (r2
) was not less than 0.999
for all drugs. The mean percent recovery of the drugs from tablet placebo at 50%, 100% and 150% were within
limits. The marketed formulations of the drugs were analyzed and the mean assay results were found to be
within limits. The developed method can thus be employed for routine simultaneous analysis of Metolazone,
Indapamide, Nebivolol, Rosuvastatin, Olmesartan and Spironolactone in bulk and in their marketed
formulations
Similar to Analytical method development and validation for residual solvent of Diltiazem hydrochloride extended release capsule by Gas chromatography (20)
Patient compliance: Challenges in management of cardiac diseases in Kuala Lum...pharmaindexing
Background
The objective of this study was to investigate the degree of compliance among cardiac patients who attend the health facilities in Kuala Lumpur and Perak, Malaysia. The reasons for non-compliance and recommendations from healthcare professionals were also evaluated.
Method
A cross-sectional study of 400 patients and 100 healthcare professionals was carried out. This study utilizes variables on external factors and internal factors as the measurement tools. The questionnaire which consists of Morisky self-reported medication adherence questions was administered to patients and causes for non-compliance sought. Questionnaire for healthcare professionals was used to determine strategies that can improve compliance rate.
Results
The study revealed a 15.8% of high adherence rate, 54.3% of moderate adherence rate and 30% of poor adherence to cardiovascular disease medications. The chi-square tests showed the strong association between dependent and independent variables. The model chosen for testing the patient compliance through external and internal factors gives an R2 value of 85.0% with an adjusted R2 of 84.7%. The F value (317.187) was also significant (p=0.000) which means that the variables have better fit in the multivariate model. The major reasons determined for non-adherence were attitudes and beliefs, lifestyle, side effects and cost of medications. The study recommends that pharmacists and dispensing technicians should be adequately qualified to provide proper counselling to cardiac patients on their medicines and disease conditions.
Conclusion
The result of this study is of value to health care providers. Compliance to cardiovascular medications will avoid treatment failures encountered in therapy.
Overview on Recurrence Pregnancy Loss etiology and risk factorspharmaindexing
Recurrent pregnancy loss (RPL) can be defined as more than two to three consecutive miscarriages before 20 weeks’ gestation; it affects approximately 1% to 2% of women. RPL is a multifactorial disease. It is very important to study the etiology and risk factors of RPL to find the best diagnostic tests and suitable therapeutic intervention. This article will discuss the current understanding etiologies and risk factors of RPL.
Novel treatments for asthma: Corticosteroids and other anti-inflammatory agents.pharmaindexing
Asthma management is a challenge due to the prevalence of disease in the world. Based on the immunological and inflammatory mechanisms of asthma, corticosteroids and anti-inflammatory participate greatly in the treatment plan. Due to different reasons, there is still an unmet need to develop new agents in this field. A lot of compounds with anti-inflammatory effect are investigated in both pre-clinical and clinical studies.
A review on liver disorders and screening models of hepatoprotective agentspharmaindexing
The liver is a vital organ present in vertebrates and some other animals. It has a wide range of functions, including detoxification, protein synthesis, and production of bio chemicals necessary for digestion. The liver is necessary for survival; there is currently no way to compensate for the absence of liver function long term, although liver dialysis can be used short term.
Carbamazepine induced Steven Johnson syndrome: A case reportpharmaindexing
Drugs are the most common cause that induces Steven Johnson syndrome (SJS) and includes antiepileptic drugs, antiretroviral drugs, anti-tuberculosis drugs, Sulphonamides, fluoroquinolones, penicillins, non-Steroidal anti-inflammatory drugs, Multivitamins. The genetic markers are also the cause for carbamazepine induced Steven Johnson Syndrome. In our study, the antiepileptic drug (Carbamazepine) is the cause for Steven Johnson Syndrome. A female patient aged 25 years came to the hospital with the complaints of bubbling over the skin and all over the body with papillary vesicles associated with pain and irritation, fever, myalgia, and nausea. The patient is known case of Phenytoin induced Steven Johnson Syndrome. In this case the patient developed the Steven Johnson Syndrome approximately after one month after starting the carbamazepine.By the withdrawal of the drug, the condition of the patient was improved.
Monoherbal formulation development for laxative activitypharmaindexing
The Ayurvedic Pharmacopoeia specifically approves flaxseed as a poultice for boils externally and demulcent or laxative internally. In this study monoherbal formulation development for laxative activity of flaxseed was undertaken. The plantLinumusitatissimumhasshowed higher percentage of total ash as well as alcohol soluble extractive values. The aqueous extract of Linumusitatissimumwas prepared by using pilot scale extraction plant and spray drying unit. The qualitative phytochemical studies reveal the presence of amino acids, carbohydrates, vitamins and proteins. From the available literatures it was found that Linumusitatissimum contains more number of amino acids. The formulated tablets showed acceptable pharmacopoeial limits and complies with specifications for thickness, hardness, friability and weight variation. The formulation has showed better laxative activity indicating additive property of the combined phytoconstituents of the plant.
Monoherbal formulation development for laxative activitypharmaindexing
The Ayurvedic Pharmacopoeia specifically approves flaxseed as a poultice for boils externally and demulcent or laxative internally. In this study monoherbal formulation development for laxative activity of flaxseed was undertaken. The plantLinumusitatissimumhasshowed higher percentage of total ash as well as alcohol soluble extractive values. The aqueous extract of Linumusitatissimumwas prepared by using pilot scale extraction plant and spray drying unit. The qualitative phytochemical studies reveal the presence of amino acids, carbohydrates, vitamins and proteins. From the available literatures it was found that Linumusitatissimum contains more number of amino acids. The formulated tablets showed acceptable pharmacopoeial limits and complies with specifications for thickness, hardness, friability and weight variation. The formulation has showed better laxative activity indicating additive property of the combined phytoconstituents of the plant.
Pneumonia and respiratory failure from swine origin influenza H1n1pharmaindexing
Swine influenza (swine flu) became alarming health concern when World Health Organization declared as “public health emergency of international concern” on April 25, 2009. After documentation of human-to-human transmission of the virus in at least three countries of two WHO regions, the WHO raised the pandemic level to 6.1 During the 1918, flu pandemic infected one-third of the world's population (an estimated 500 million people) and caused approximately 50 million deaths.2 In 1976, an outbreak of swine influenza occurred in New Jersey, USA, which involved more than 200 cases, some of them severe, resulting in one death.3 In 1988, another fatality was reported as a complication of swine influenza.
A descriptive study on newborn care among postnatal mothers in selected mater...pharmaindexing
The newborn health challenge faced by India is more formidable than that experienced by any other country in the world. The newborn health is inevitably affected by the traditional care practices of the mothers causing high infant morbidity and mortality.The aim of the study were determine the knowledge, attitude and practice of postnatal mothers regarding new born care and find out the association between knowledge, attitude and practice of postnatal mothers regarding new born care and to determine the association between these as well as with the selected demographic variables. A descriptive study was conducted to assess the knowledge, attitude and practice of postnatal mothers regarding new born care in selected maternity centres in Madurai. Survey approach was employed to select sample and it consisted of 100 postnatal mothers. Data was collected using structured interview schedule. Findings of the study showed that 65% of postnatal mothers had moderate knowledge; 61% had favourable attitude and 57% of them had high practice of new born care. There was a significant association between knowledge and attitude (r=+0.567), knowledge and practice (r=+0.388), attitude and practice (r=+0.321) .There was a significant association between knowledge and education, monthly family income and obstetrical score at p<0.05. Findings of the study indicated the need to conduct frequent assessment of knowledge, attitude and practice of postnatal mothers regarding new born care. Awareness and attitude of the mothers towards new born care still has lots of lacunae especially in those who belong to the lower socio economic statusand poorly educated postnatal mothers. So it is imperative to provide comprehensive training in the field of new born care for mothers during pregnancy
Late 19th century was evident of intelligent biomaterial; which has changed researcher’s perspective towards science and technology. This intelligent biomaterial are envisioned to have huge impact on Healthcare from sequential signalling of biomedical molecule, mimicking natural gene, an effective drug carrier, to high resolution diagnostic tool.From drug discovery aspect many of NCE fail to reach therapeutic potential due to PK/ PD profile. Nanotechnology has changed the face of drug discovery form chemical evaluation to structure of proteins in signalling pathways and development of chemical antibody. Nanotechnology from lab to market approval is long process due to regulatory evaluation. Though it seems to be bright future market it has to go through a long process from being innovation to complete market product. This makes whole process expensive making investor reluctant to invest in big projects.Western world is aware of dramatic potential of nano-projects; which has its limitation in financial investments; with major challenge of transforming nano science to commercial pharmaceutical product.
The Flaws in health practice in post-operative management of a patient in ter...pharmaindexing
Introduction
Congenital urinary tract obstructions are common cause of kidney damage sometimes which sometimes presents itself without symptoms leading to abnormalities in blood filtration and consequently retarded kidney function. A cohort study was conducted in such patient to find out the short comings in treatment strategy.
Case presentation
A four years old child, weighing 14 kg was brought with severe constipation, fever, chest congestion and cough later developed left eye disorientation after admission to hospital, diagnosed with urinary tract obstruction, indicating acidosis and loss of electrolytes due to excessive loss of water. His therapy management included surgical treatment, dialysis and to improve his electrolyte levels within the normal with the treatment chest congestion and fever.
Conclusion
This case study reports the post operative treatment of congenital urinary tract obstructions in a tertiary care hospital and highlights the discrepancies observed. Antibiotic rationality and irrational prescribing was observed. The case study highlights the need of a clinical pharmacist in the health care team.
Corticosteroid induced disorders – An overviewpharmaindexing
Glucocorticoids are important in the treatment of many inflammatory, allergic, immunologic, and malignant disorders, and the toxicity of glucocorticoids is one of the commonest causes of iatrogenic illness associated with chronic inflammatory disease.Glucocorticoid-induced muscle atrophy is characterized by fast-twitch or type II muscle fiber atrophy. Corticosteroid (CS) therapy is widely used in the treatment of rheumatic diseases.Osteoporosis remains one of its major complications.Steroid induced glaucoma is a form of open angle glaucoma occurring as an adverse effect of corticosteroid therapy. Glucocorticoids induce hepatic and extrahepatic insulin resistance.Glucocorticoid treatment impairs both glucose transport in fat and muscle cells. Corticosteroid-induced psychosis represents a spectrum of psychological changes that can occur at any time during treatment. Cushing’s syndrome describes the signs and symptoms associated with prolonged exposure to inappropriately high levels of the hormone cortisol. Physicians must be aware of these adverse effects and be equipped to manage them.
Anti-inflammatory activity of pupalia lappacea L. Jusspharmaindexing
Pupalia lappacea (L) Juss is an erect shrub used in folklore medicine to treat bone fractures and in inflammatory conditions. Methanolic extract of aerial parts shown is claimed in traditional medicine that the leaves of the plant are used in the treatment of inflammation. In the present study, the methanolic extract of Pupalia lappacea was screened for its anti-inflammatory activity using carageenan induced rat paw edema egg white induced paw oedema models. The methanolic extract at the dose of 200 mg/kg p.o exhibited significant anti-inflammatory activity in carrageenan induced paw edema model (p<0.01). In egg white induced model, methanolic extract at the dose of 200 mg/kg inhibited paw oedema significantly (p<0.01) indicating that both test samples inhibit the increase in number of fibroblasts and synthesis of collagen and mucopolysaccharides during prostaglandin formation during the inflammation. These experimental results have established a pharmacological evidence for the folklore claim of the drug to be used as an anti inflammatory agent. HPTLC analysis of the extract shows the presence of gallic acid 1.24mg/ml, ferulic acid 2.00mg/ml, chlorogenic acid 46.25mg/ml and rutin 7.02mg/ml of the extract which were responsible for the claimed anti-inflammatory action in the animal models studied.
Lucinactant: A new solution in treating neonatal respiratory distress syndrom...pharmaindexing
Lucinactant is a novel synthetic surfactant, approved by the FDA on March 6th 2012, for use in treatment of RDS. It’s superiority as compared to the previously approved surfactants lie in containing sinapultide, a 21-amino acid peptide also known as KL4 peptide, which has been designed to mimic the activity of human surfactant protein. Lucinactant is completely devoid of any animal derived components. It is the fifth drug approved by the FDA for the treatment of RDS. It has shown immense efficacy in phase two clinical trials and animal model studies and exhibited better efficiency when compared to other surfactants in both 24 hour and two week mortality rates of infants in RDS. Lucinactant tends reduce the surface tension at the air-liquid interface of alveolar surfaces and allows lungs to function normally. It was observed that the side effects were lesser with Lucinactant when compared with other naturally derived surfactants.
Bioactivity screening of Soil bacteria against human pathogenspharmaindexing
Microorganisms have a profound effect on medical science as they not only infect & cause disease but also produce metabolic products that can cure infections. Soil happens to be a source for a variety of microorganisms. Most of the bacteria, particularly actinomycetes produce biologically active secondary metabolites. Though there are a number of antibiotics available, there is a pressing need for the discovery of new source for antimicrobials against the pathogens due to the development of drug resistance of the pathogenic microorganisms. In addition to, new pathogenic strains are also developing and causing infection to human beings. Bioactive compounds are compounds that are produced by any living organism and are known to exhibit various biological activities both in-vitro & in-vivo. Bioactivity may be antimicrobial, antineoplastic, anticancerous, immunomodulation, antifertility & others. Soil bacteria were isolated by standard technique and by making use of selective media. The isolates were identified and subjected for preliminary screening to look for their ability to produce bioactive materials. A total of 96 strains were isolated from three different soil samples. 14 of them were found to have antibacterial activity against the human pathogens like Staphylococcus aureus, Streptococcus faecalis, E.coli, Klebsiella aerogenes, Proteus vulgaris, Pseudomonas aureginosa and Salmonella typhi by preliminary screening. Further the selected (3) bacteria were grown in the suitable culture media for the production of bioactive metabolites by using rotary shake flask. The active metabolites was isolated by solvent extraction and concentrated by evaporation under reduced pressure. The antimicrobial screening of the active metabolites showed prominent effect against the clinical pathogens under the study.
A study on sigmoid Volvulus presentation and managementpharmaindexing
A study on sigmoid volvulus presentation and management was a 2yr retrospective study done at RMMCH.The diagnosis of sigmoid volvulus was made from a history of large bowel obstruction (constipation, abdominal distension, and abdominal pain), which were often recurrent and plain abdominal radiographs.The morbidity associated isSuperficial wound infection occurred in four patients. All the infected wounds eventually healed with conservative measures. Clinical anastomotic dehiscence was noted in 1 patient for which during relaparotomy proximal colostomy and mucous fistula was done. The mortality associated is shown is there were 9 deaths of which 7 were due to sepsis and 2 were due to comorbid illness. Two out of eight patients for whom a colopexy was done had a recurrent attack of sigmoid volvulus. The duration of hospital stay ranged between 10 and 21 days. Use of sigmoidoscopic detorsion for viable colon should be encouraged. Sigmoidopexy, which is associated with a recurrence rate of 20% in our series of patients, should be used selectively.Hartmann’s procedure is a safe option in sigmoid volvulus with gangrenous bowel. Primary anastomosis in emergency situation can be carried out with morbidity and mortality in patients with viable colon
Evaluation of Preliminary phytochemical on various some medicinal plantspharmaindexing
The present study was carried out to evaluate the physical status and percentage yield of methanolic extract and its fractions of whole plant of Leucas cephalotes, leaves of Hiptage benghalensis and leaves of Kydia calycina were recorded for future references and Preliminary phytochemical screening of MLC, MHB and MKC revealed the presence of carbohydrates, glycosides, saponins, flavonoids, steroidal and phenolic compounds. MLC revealed the presence of all the above mentioned phytoconstituents except saponins and also MKC steroidal compounds. The fractions of MLC, MHB and MKC revealed the presence of glycosides, phenolic compounds, steroids and flavonoids.
Comparision of in vitro antibacterial activity of cefoperazone and levofloxac...pharmaindexing
Cefoperazone (a third generation cephalosporin) has effective in vitro activity against majority of pathogens. Levofloxacin (a flouroquinolone) is one which prescribed more due to its increased antibacterial activity against Gram-positive, Gram-negative, and atypical bacteria. Microbial resistance to antibiotics is now prevalent and poses a serious clinical threat. An attempt has been made to evaluate sensitivity of Cefoperazone and Levofloxacin against Escherichia coli, Staphylococcus aureus, Pseudomonas aeruginosa and Salmonella typhi. A total of 120 isolates were collected from different pathological laboratories and medical centers in Karachi, Pakistan. The above stated clinical isolates were extracted from urine/stool, skin, blood and sputum samples. Results show least resistance of Levofloxacin as compare to Cefoperazone against Escherichia coli (32.5% and 42.5%) and Pseudomonas aeruginosa (36% and 48%) while Staphylococcus aureus is still susceptible towards Cefoperazone and least sensitive to Levofloxacin by showing 26.6% and 50% resistance respectively. Study concluded that the prevalent pathogens are still susceptible towards Levofloxacin and Cefoperazone but the gradual increase in resistance is alarming to the general practice of prescribing antibiotic which require routine evaluation and surveillance to ensure the effectiveness of the antibacterial agents.
Concept of srotas from ayurvedic perspective with special reference to neurologypharmaindexing
Ayurveda is a life science. The researchers of ayurveda could rule out the presence of srotas (channels) spreading throughout the human body. These srotas (channels) are governed by vayu which is using all the srotas (channels) of the body to carry out the functional and physiological activities of the human body without which the human society will not exist. Several synonymous words have been described by the ayurvedicacharyas for srotas. Some are micro and some are macro in structures and they adopt the same colour of the particular dhatus of the body to which it belongs. The aim of the study is to justify that srotas are nothing but innurmerable channels or pathways of the nervous system governed by electric current without which no functional and physiological activities of the human body will develope.
Health promotion survey in overweight and obese students of universities in n...pharmaindexing
Introduction
Overweight and obesity is one of the major health problems in the UK and worldwide. Approximately two-thirds of the population in the UK is either overweight or obese. Overweight and obesity is an important issue that causes distress to most women. Health promotion is the best method to educate overweight and obese women. It is defined as the process enabling people to increase control over and to improve their health by Ottawa Charter for Health Promotion. It is aimed to enhance the well-being of the individuals and their positive attitudes towards prevention of various diseases. In order to make any improvement to the health promotion for overweight and obesity, the risk factors and the opinions from the public should first be identified and addressed.
Methods
Cross-sectional survey design was selected with a questionnaire that consisted of 20 open and close ended questions. A sample size of 196 was determined. The data thus gathered was analyzed using SPSS V20 (Statistical Package for Social Science version 20). Descriptive statistics (fx) and (SD) were used and Chi-square X2 test for association was employed.
Results
Out of the total 196 responses, only (40%) of the students had normal weight (SD 1.1), (25%) students had a good understanding of health promotion (SD 1.6), half (50%) appeared concerned about their weight (SD 0.5), (60%) had an obese family member (0.5). The BMI of students was associated with the presence of an obese member in their family and their weight as a concern for them. (P-value <0.05).
Conclusion
The health promotion service is beneficial as it was found to have raised concerns in the mind of the students regarding over weight and obesity. However it was observed that the understanding of health promotion service was different among students and this is the root of the problem.
Report Back from SGO 2024: What’s the Latest in Cervical Cancer?bkling
Are you curious about what’s new in cervical cancer research or unsure what the findings mean? Join Dr. Emily Ko, a gynecologic oncologist at Penn Medicine, to learn about the latest updates from the Society of Gynecologic Oncology (SGO) 2024 Annual Meeting on Women’s Cancer. Dr. Ko will discuss what the research presented at the conference means for you and answer your questions about the new developments.
ARTIFICIAL INTELLIGENCE IN HEALTHCARE.pdfAnujkumaranit
Artificial intelligence (AI) refers to the simulation of human intelligence processes by machines, especially computer systems. It encompasses tasks such as learning, reasoning, problem-solving, perception, and language understanding. AI technologies are revolutionizing various fields, from healthcare to finance, by enabling machines to perform tasks that typically require human intelligence.
Explore natural remedies for syphilis treatment in Singapore. Discover alternative therapies, herbal remedies, and lifestyle changes that may complement conventional treatments. Learn about holistic approaches to managing syphilis symptoms and supporting overall health.
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!
Prix Galien International 2024 Forum ProgramLevi Shapiro
June 20, 2024, Prix Galien International and Jerusalem Ethics Forum in ROME. Detailed agenda including panels:
- ADVANCES IN CARDIOLOGY: A NEW PARADIGM IS COMING
- WOMEN’S HEALTH: FERTILITY PRESERVATION
- WHAT’S NEW IN THE TREATMENT OF INFECTIOUS,
ONCOLOGICAL AND INFLAMMATORY SKIN DISEASES?
- ARTIFICIAL INTELLIGENCE AND ETHICS
- GENE THERAPY
- BEYOND BORDERS: GLOBAL INITIATIVES FOR DEMOCRATIZING LIFE SCIENCE TECHNOLOGIES AND PROMOTING ACCESS TO HEALTHCARE
- ETHICAL CHALLENGES IN LIFE SCIENCES
- Prix Galien International Awards Ceremony
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.
Title: Sense of Smell
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 primary categories of smells and the concept of odor blindness.
Explain the structure and location of the olfactory membrane and mucosa, including the types and roles of cells involved in olfaction.
Describe the pathway and mechanisms of olfactory signal transmission from the olfactory receptors to the brain.
Illustrate the biochemical cascade triggered by odorant binding to olfactory receptors, including the role of G-proteins and second messengers in generating an action potential.
Identify different types of olfactory disorders such as anosmia, hyposmia, hyperosmia, and dysosmia, including their potential causes.
Key Topics:
Olfactory Genes:
3% of the human genome accounts for olfactory genes.
400 genes for odorant receptors.
Olfactory Membrane:
Located in the superior part of the nasal cavity.
Medially: Folds downward along the superior septum.
Laterally: Folds over the superior turbinate and upper surface of the middle turbinate.
Total surface area: 5-10 square centimeters.
Olfactory Mucosa:
Olfactory Cells: Bipolar nerve cells derived from the CNS (100 million), with 4-25 olfactory cilia per cell.
Sustentacular Cells: Produce mucus and maintain ionic and molecular environment.
Basal Cells: Replace worn-out olfactory cells with an average lifespan of 1-2 months.
Bowman’s Gland: Secretes mucus.
Stimulation of Olfactory Cells:
Odorant dissolves in mucus and attaches to receptors on olfactory cilia.
Involves a cascade effect through G-proteins and second messengers, leading to depolarization and action potential generation in the olfactory nerve.
Quality of a Good Odorant:
Small (3-20 Carbon atoms), volatile, water-soluble, and lipid-soluble.
Facilitated by odorant-binding proteins in mucus.
Membrane Potential and Action Potential:
Resting membrane potential: -55mV.
Action potential frequency in the olfactory nerve increases with odorant strength.
Adaptation Towards the Sense of Smell:
Rapid adaptation within the first second, with further slow adaptation.
Psychological adaptation greater than receptor adaptation, involving feedback inhibition from the central nervous system.
Primary Sensations of Smell:
Camphoraceous, Musky, Floral, Pepperminty, Ethereal, Pungent, Putrid.
Odor Detection Threshold:
Examples: Hydrogen sulfide (0.0005 ppm), Methyl-mercaptan (0.002 ppm).
Some toxic substances are odorless at lethal concentrations.
Characteristics of Smell:
Odor blindness for single substances due to lack of appropriate receptor protein.
Behavioral and emotional influences of smell.
Transmission of Olfactory Signals:
From olfactory cells to glomeruli in the olfactory bulb, involving lateral inhibition.
Primitive, less old, and new olfactory systems with different path
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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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Analytical method development and validation for residual solvent of Diltiazem hydrochloride extended release capsule by Gas chromatography
1. Raja Sundararajan et al / Int. J. of Pharmacy and Analytical Research Vol-2(4) 2013 [194-203]
194
*Corresponding author: Raja Sundararajan
E-mail address: sraja61@gmail.com
IJPAR |Volume 2 | Issue 4 | Oct - Dec-2013 ISSN: 2320-2831
Available Online at: www.ijpar.com
[Research article]
Analytical method development and validation for residual solvent of
Diltiazem hydrochloride extended release capsule by Gas chromatography
*
Raja Sundararajan, Christopher Vasanth Kumar, Jayaveera.
Gitam institute of Pharmacy, Gitam university, visakhapatnam -530045, Andrapradesh, India.
ABSTRACT
Residual solvents are organic volatile chemicals that are either used or produced during the manufacture of
active pharmaceutical ingredients, excipients, and drug products. Organic solvents such as di ethyl ether, N
heptane, acetone, methyl acetate, tertiary - butyl alcohol, iso-propyl alcohol, ethanol , toluene, Nbutanol, and n-
butyl acetate frequently used in pharmaceutical industry for the manufacturing of drug product Gas
Chromatography method for the determination of residual solvent of Diltiazem Hydrochloride Extended
Release Capsulesfor iso-propyl alcoholhas been carried out using this method.this method utilizedPerkin Elmer
clarus 580 GC Turbomatrix 40 Headspace sampler and DB-624, 30 m x 0.530 mm ID, 3.0 µm column was used
with flame ionizationdetector (FID). The GC method for the determination of residual solvent of Diltiazem
Hydrochloride Extended Release Capsules was validated. The method was found to be specific, precise, linear,
accurate, rugged, robust and suitable for its intended use.
Keywords: Diltiazem Hydrochloride, iso-propyl alcohol, ICH, validation.
INTRODUCTION
Diltiazem is a calcium ion influx inhibitor (slow
channel blocker or calcium antagonist).
Chemically, diltiazem hydrochloride is 1, 5-
Benzothiazepin-4(5H) one, 3-(acetyloxy)-5-[2-
(dimethylamino)ethyl]-2,3-dihydro-2-(4-methoxy
phenyl)-, mono hydrochloride, (+)-cis-. Its
molecular formula is C22H26N2O4S HCl and its
molecular weight is 450.99. Diltiazem produces its
antihypertensive effect primarily by relaxation of
vascular smooth muscle with a resultant decrease in
peripheral vascular resistance. The magnitude of
blood pressure reduction is related to the degree of
hypertension; thus hypertensive individuals
experience an antihypertensive effect, whereas
there is only a modest fall in blood pressure in
normotensives. International Conference on
Harmonization (ICH) [1-2]
. General chapter in USP
[3]
.Gas chromatography method for the
determination of residual solvents[4-5]
. Analytical
Methods for Residual Solvents Determination in
Pharmaceutical Products and excipients[6-7]
.
Chromatographic methods for residual solvents
analysis for iso propyl alcohol[8-9]
. A review on
GC-MS and Method Development and
Validation[10]
. Since this drug is official in
pharmacopoeia only in dissolution method.No
previous GC-FID method for the determination and
quantification of Diltiazem Hydrochloride
Extended Release Capsules in literature. Therefore,
the purpose of this investigation was to develop
and validate a method using a simple, rapid,
sensitive, specific, precise, linear, accurate, rugged,
robust GCFID method.
2. Raja Sundararajan et al / Int. J. of Pharmacy and Analytical Research Vol-2(4) 2013 [194-203]
195
MATERIALS AND METHOD
Reagents/chemicals
Isopropyl alcohol : GC/HPLC/GR
Dimethyl sulphoxide : HPLC Grade
GC conditions
Instrument : Gas chromatography with Headspace
Column : DB624, 30m x 0.530 mm ID x 3.0 µm
Carrier gas : Nitrogen
Linear velocity : 35 cm/sec
Detector : 240°C, FID
Range : 1
Attenuation : 4
Injector temperature : 200 °C
Oven temperature program :
Temperature : 40°C
Hold time ‘1’ : 0°C/min
Rate temp : 10°C/min
Hold temp : 220°C
Hold Time ‘2’ : 5 min
Run time : 23 min
Gas flow : Constant velocity
Split : 1:20
Hydrogen : 45 mL/min
Zero Air : 450 mL/min
Condition for Head Space Sampler
Vial temperature : 100 °C
Needle temperature : 110 °C
Transfer line temperature : 120 °C
Injection volume : 0.06 mL
Thermostat : 15 min
High pressure inject : on
Head space mode : constant
Carrier gas pressure : 15 psi
Vial pressurization : 4 min
Withdraw time : 0.2 min
GC cycle time : 35 min
Solution preparation
Blank solution
Transfer 4.0 mL of Dimethyl sulphoxide in
headspace vial and seal it using vial crimper.
Standard stock solution
To a 100.0 mL volumetric flask containing 20.0
mL of Dimethyl sulphoxide, transfer about 250.0
mg of Isopropyl alcohol (IPA) dilute to volume
with Dimethyl sulphoxide and mix well.
Standard solution
Transfer 25.0 mL of standard stock solution into
100 mL volumetric flask, dilute to volume with
Dimethyl sulphoxide and mix.
Transfer 4.0 mL of the standard solution into a
head space vial, and seal it using vial crimper.
3. Raja Sundararajan et al / Int. J. of Pharmacy and Analytical Research Vol-2(4) 2013 [194-203]
196
Test solution
Crush the pellets in to fine powder. Transfer 500
mg of powdered sample in a headspace vial. Add 4
mL of Dimethyl sulphoxide and seal it using vial
crimper.
LOD, LOQ and retention time data*
Name LOD (ppm) LOQ (ppm)
Isopropylalcohol
alcohol
25 80
*LOD, LOQ data incorporated after method validation.
Calculation
Isopropyl
alcohol content
in ppm
=
AT
x
CS
x
P
x 106
AS CT 100
Where,
AT : Area of Isopropyl alcohol peak in
the chromatogramof sample
solution.
AS : Average area of Isopropyl alcohol
peak in the chromatogram of
standard solution.
CS : Concentration of standard solution
in mg/mL
CT : Concentration of sample solution in
mg/mL
P : Percentage purity of standard.
RESULTS AND CONCLUSIONS
PRECISION
SYSTEM PRECISION
Six replicate injections of standard solution were
injected. The mean and percentage relative
standard deviation (% RSD) for peak areas were
calculated. The results are tabulated in table - 1.
Acceptance criteria
Percentage relative standard deviation (% RSD) for
peak areas is not more than 10.0
METHOD PRECISION
Six samples of 360 mg capsuleswere prepared by
spiking the residual solvent at specification level
and analysed as per test method. The residual
solvent content in six samples and percentage
relative standard deviation (% RSD) for six results
were calculated and the results are tabulated in
table-2.
Acceptance criteria
The percentage relative standard deviation (%
RSD) for content of residual solvent from six
samples is not more than 15.0.
INTERMEDIATE PRECISION
(RUGGEDNESS)
Ruggedness of the method was verified by
analysing the six samples spiked with residual
solvent at specification level from the same batch
which was used for method precision as per test
method by different analyst, different lot no. of
column, and different instrumentation different
day. The content of residual solventswas
determined. Calculated percentage relative standard
deviation (% RSD) for residual solventin six
samples and also calculated overall percentage
relative standard deviation (% RSD) for ruggedness
results with the method precision results. The
results are tabulated in table-3.
Acceptance criteria
The percentage relative standard deviation (%
RSD) for residual solvent contentfrom six samples
is not more than 15.0. Overall percentagerelative
standard deviation (%RSD) for method and
intermediate precision results is not more than 15.0
SPECIFICITY
Blank, placebo, standard, sample solution and
sample solution spiked with residual solvent at
specification level were injected. The elution
pattern in blank and placebo observed. The
retention time of analyte peak from standard
solution and sample (spiked) are compiled in table-
4. 197
Raja Sundararajan et al / Int. J. of Pharmacy and Analytical Research Vol-2(4) 2013 [194-203]
197
4. Refer figure 2 to 6 for the chromatograms of
blank, placebo, standard, sample and spiked sample
Acceptance criteria
Observe the elution of peak pattern in the blank and
placebo.
$- Refer retention time for standard and sample
solution from method precision experiment.
LIMIT OF DETECTION AND LIMIT OF
QUANTITATION
(LOD and LOQ)
The limit of detection (LOD) and limit of
quantitation (LOQ) was determined for Isopropyl
alcoholby signal to noise ratio method by using the
formula.
Signal to noise ratio (S/N) = 2H/h
H - Height of analyte
h - Height of noise
LOQ value was verified by giving six replicate
injections of solution containing Isopropyl alcohol.
LOD and LOQ values are summarized in table -5a.
The percentage relative standard deviation (%
RSD) calculated for peak areas and tabulated in
table-5b
Acceptance criteria
Signal to noise ratio 10:1 at the level of LOQ and
2:1 or 3:1 at the level of LOD.
The percentage relative standard deviation (%
RSD) for peak areas at LOQ level is not more than
15.0
LINEARITY
Linearity for Isopropyl alcohol was performed
from about LOQ to 150 % level. A graph was
plotted with concentration (in ppm) on x-axis and
peak areas on y-axis. Slope, y-intercept, correlation
coefficient and residual sum of squares (RSS) were
determined. The results are tabulated in table -6
graphically represented in figure- 1
Acceptance criteria
The correlation coefficient (r-value) value is not
less than 0.97
ACCURACY (RECOVERY)
Known amount of residualsolvent spiked with
sample at about LOQ, 100% and 150% of
specification limit. The percentage recovery was
calculated from the amount found and actual
amount added. The results are tabulated in table - 7.
Acceptance criteria
Percentage recovery at each level is in between
85.0 and 115.0
Percentage relative standard deviation (%RSD) is
not more than 15.0 at each level.
RANGE
Range inferred from the data of linearity, accuracy
and precision experiments.
ROBUSTNESS
Robustness of the method was verified by
deliberately varying the following condition.
i) By changing the flow rate by 10%.
System suitability was evaluated and residual
solvent spiked sample was analysed in triplicate.
Calculated cumulative percentage relative standard
deviation (% RSD) for each condition and method
precision data. The results tabulated in table-8. The
system suitability parameters are tabulated in table-
9.
Acceptance criteria
Overall percentage relative standard deviation (%
RSD) for each change condition and method
precision results is not more than ± 15.0
SUMMARY OF SYSTEM SUITABILITY
System suitability was evaluated by injecting
standard solution during various days of validation.
The percentage relative standard deviation (%
RSD) for the peak areas were verified. The results
are tabulated in table – 9
Acceptance Criteria
The percentage relative standard deviation (%
RSD) for the six injections of standard is not more
than 10.0
5. Raja Sundararajan et al / Int. J. of Pharmacy and Analytical Research Vol-2(4) 2013 [194-203]
198
TABLES
TABLE – 1-SYSTEM PRECISION
Injection No. Peak area
1 187952
2 191760
3 189915
4 188706
5 188366
6 192441
Mean 189857
% RSD 1.0
TABLE – 2-METHOD PRECISION
Sample No. Isopropyl alcohol (ppm)
1 6125
2 6284
3 6171
4 6097
5 6145
6 6118
Mean 6157
% RSD 1.1
TABLE – 3-INTERMEDIATE PRECISION
Sample No. Isopropyl alcohol (ppm)
Analyst 1 Analyst 2
1 6125 6280
2 6284 6101
3 6171 6266
4 6097 6205
5 6145 6345
6 6118 6487
Mean 6157 6281
Percentage relative
standard deviation (%
RSD)
1.1 2.1
Overall average 6219
Over all Percentage
relative standard deviation
(% RSD)
1.9
6. 199
Raja Sundararajan et al / Int. J. of Pharmacy and Analytical Research Vol-2(4) 2013 [194-203]
199
TABLE – 4-SPECIFICITY
Peak Name Sample type RT (min.) $
Isopropyl alcohol Standard 3.159
Spiked sample 3.157
TABLE -5a-SUMMARY OF LOD AND LOQ VALUES
Name LOD LOQ
ppm S/N ppm S/N
Isopropyl alcohol 25 27 80 68
TABLE -5b-PRECISION AT LOQ
Injection No. Peak area
1 3018
2 2924
3 2976
4 2949
5 2966
6 2994
Mean 2971
% RSD 1.1
S/N - Signal to noise ratio
TABLE –6-LINEARITY OF ISOPROPYL ALCOHOL
Level (%) Concentration in ppm Peak area
LOQ 80.0384 2956
25 1250.6000 45189
50 2501.2000 90831
75 3751.8000 138527
100 5002.4000 185430
125 6253.0000 237433
150 7503.6000 285464
Slope 38.1514
y-intercept -2739.8875
Correlation coefficient 0.99978
Residual sum of squares 17614806.9169
7. Raja Sundararajan et al / Int. J. of Pharmacy and Analytical Research Vol-2(4) 2013 [194-203]
200
TABLE –7-ACCURACY OF ISOPROPYL ALCOHOL
Level Amount found in µg Actual amount added in µg % Recovery
Mean % RSD
Level - 1
(LOQ)
70.7097 79.9584 88.4 95.7 12.9
70.9501 79.9584 88.7
87.8531 79.9584 109.9
Level - 2
(100%)
5184.0542 4997.3976 103.7 105.3 1.9
5377.5980 4997.3976 107.6
5233.5884 4997.3976 104.7
Level - 3
(150%)
7710.7255 7496.0964 102.9 101.3 1.4
7526.1539 7496.0964 100.4
7544.0716 7496.0964 100.6
TABLE –8-ROBUSTNESS
S.No. Method precision Flow rate (31.5 cm/sec) Flow rate
(38.5cm/sec)
1 6125 5654 5600
2 6284 5654 5605
3 6171 5795 5765
4 6097 - -
5 6145 - -
6 6118 - -
Mean 6157 - -
%RSD 1.1 - -
Overall Mean - 6005 5990
Overall %RSD - 4.0 4.3
TABLE -9-SUMMARY OF SYSTEM SUITABILITY
S.No Name of Experiment % RSD
1 System precision and
Method precision
1.0
2 Specificity and Robustness 0.6
3 Robustness
(Flow Rate – 38.5 cm/Sec)
0.6
4 Robustness
(Flow Rate – 31.5 cm/Sec)
1.0
5 LOQ, LOD, Linearity and Accuracy 0.8
6 Intermediate Precision 1.8
8. 201
Raja Sundararajan et al / Int. J. of Pharmacy and Analytical Research Vol-2(4) 2013 [194-203]
201
FIGURES
Figure 1: Linearity plot for Isopropyl alcohol
Figure - 2: Chromatogram of blank
Figure - 3: Chromatogram of placebo
0
50000
100000
150000
200000
250000
300000
0.0000 2000.0000 4000.0000 6000.0000 8000.0000
Area
Concentration µg/mL
Isopropyl alcohol
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Figure - 4: Chromatogram of standard
Figure - 5: Chromatogram of sample (unspiked)
Figure - 6: Chromatogram ofspiked sample
10. 203
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ACKNOWLEDGEMENTS
The authors are grateful to piramal health care Ltd,
India. For providing Diltiazem hydrochloride as a
gift sample.
CONCLUSION
This study presents a simple and validated Gas
chromatographic method for estimation of residual
solvents in Diltiazem Hydrochloride Extended
Release Capsule drug product. The developed
method is specific, precise, linear, accurate, rugged,
robust and suitable for its intended use.
REFERENCES
[1] ICH Expert Working Group. Impurities: Guideline for Residual solvents. Q3C[R5],
2011.
[2] ICH. Validation of Analytical Procedures, Text and Methodology, Q2 (R1), 2005.
[3] USP <467> Residual solvents.
[4] Marie-JoséeRocheleau, MélanieTitley, Julie Bolduc, Measuring residual solvents in pharmaceutical
samples using fast gas chromatography techniques, Journal of Chromatography B, 805, 2004, 77–86.
[5] Chusena Narasimharaju Bhimanadhuni and Devala Rao Garikapati, Development and validation of gas
chromatography method for the determination of residual solvents in Mirabegron,Der PharmaChemica,
2013, 5(1):55-60.
[6] Katarzyna Grodowska and Andrzej Parczewski, Analytical Methods For Residual Solvents
Determination In Pharmaceutical Products, Acta Poloniae Pharmaceutica ñ Drug Research, Vol. 67
No.1, 2010:13-26.
[7] RohitkumarM.Yadav and KapilPatil, Development and Validation of Gas Chromatographic Analytical
Method for Estimation of Residual Solvents in Excipients (Klucell, Triacetan, HPMC), International
Journal of Research in Pharmaceutical and Biomedical Sciences,Vol. 4 (2) Apr– Jun 2013, 618-623.
[8] Praveen Kumar Baliyan, R.P. Singh and SaurabhArora, Simultaneous Estimation of Residual Solvents
(Isopropyl Alcohol and Dichloromethane) in Dosage Form by GC-HS-FID, Asian Journal of
Chemistry, Vol. 21, No. 3 (2009), 1739-1746.
[9] S.B. Puranik, Varun R. Pawar, N. Lalitha, P.N. Sanjay Pai and G.K. Rao, Gas chromatographic
methods for residual solvents analysis, Oriental Journal of Chemistry, Vol. 24(1), 2008, 529-536.
[10]Lakshmi Hima Bindu M.R, Angala Parameswari S,Gopinath C,A Review on GC-MS and Method
Development and Validation, International Journal of Pharmaceutical Quality Assurance 2013; 4 ( 3) ;
42-51.
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*Corresponding author: Raja Sundararajan
E-mail address: sraja61@gmail.com
IJPAR |Volume 2 | Issue 4 | Oct - Dec-2013 ISSN: 2320-2831
Available Online at: www.ijpar.com
[Research article]
Analytical method development and validation for residual solvent of
Diltiazem hydrochloride extended release capsule by Gas chromatography
*
Raja Sundararajan, Christopher Vasanth Kumar, Jayaveera.
Gitam institute of Pharmacy, Gitam university, visakhapatnam -530045, Andrapradesh, India.
ABSTRACT
Residual solvents are organic volatile chemicals that are either used or produced during the manufacture of
active pharmaceutical ingredients, excipients, and drug products. Organic solvents such as di ethyl ether, N
heptane, acetone, methyl acetate, tertiary - butyl alcohol, iso-propyl alcohol, ethanol , toluene, Nbutanol, and n-
butyl acetate frequently used in pharmaceutical industry for the manufacturing of drug product Gas
Chromatography method for the determination of residual solvent of Diltiazem Hydrochloride Extended
Release Capsulesfor iso-propyl alcoholhas been carried out using this method.this method utilizedPerkin Elmer
clarus 580 GC Turbomatrix 40 Headspace sampler and DB-624, 30 m x 0.530 mm ID, 3.0 µm column was used
with flame ionizationdetector (FID). The GC method for the determination of residual solvent of Diltiazem
Hydrochloride Extended Release Capsules was validated. The method was found to be specific, precise, linear,
accurate, rugged, robust and suitable for its intended use.
Keywords: Diltiazem Hydrochloride, iso-propyl alcohol, ICH, validation.
INTRODUCTION
Diltiazem is a calcium ion influx inhibitor (slow
channel blocker or calcium antagonist).
Chemically, diltiazem hydrochloride is 1, 5-
Benzothiazepin-4(5H) one, 3-(acetyloxy)-5-[2-
(dimethylamino)ethyl]-2,3-dihydro-2-(4-methoxy
phenyl)-, mono hydrochloride, (+)-cis-. Its
molecular formula is C22H26N2O4S HCl and its
molecular weight is 450.99. Diltiazem produces its
antihypertensive effect primarily by relaxation of
vascular smooth muscle with a resultant decrease in
peripheral vascular resistance. The magnitude of
blood pressure reduction is related to the degree of
hypertension; thus hypertensive individuals
experience an antihypertensive effect, whereas
there is only a modest fall in blood pressure in
normotensives. International Conference on
Harmonization (ICH) [1-2]
. General chapter in USP
[3]
.Gas chromatography method for the
determination of residual solvents[4-5]
. Analytical
Methods for Residual Solvents Determination in
Pharmaceutical Products and excipients[6-7]
.
Chromatographic methods for residual solvents
analysis for iso propyl alcohol[8-9]
. A review on
GC-MS and Method Development and
Validation[10]
. Since this drug is official in
pharmacopoeia only in dissolution method.No
previous GC-FID method for the determination and
quantification of Diltiazem Hydrochloride
Extended Release Capsules in literature. Therefore,
the purpose of this investigation was to develop
and validate a method using a simple, rapid,
sensitive, specific, precise, linear, accurate, rugged,
robust GCFID method.](https://image.slidesharecdn.com/ijparrajasundararajan-141215071154-conversion-gate02/85/Analytical-method-development-and-validation-for-residual-solvent-of-Diltiazem-hydrochloride-extended-release-capsule-by-Gas-chromatography-1-320.jpg)
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MATERIALS AND METHOD
Reagents/chemicals
Isopropyl alcohol : GC/HPLC/GR
Dimethyl sulphoxide : HPLC Grade
GC conditions
Instrument : Gas chromatography with Headspace
Column : DB624, 30m x 0.530 mm ID x 3.0 µm
Carrier gas : Nitrogen
Linear velocity : 35 cm/sec
Detector : 240°C, FID
Range : 1
Attenuation : 4
Injector temperature : 200 °C
Oven temperature program :
Temperature : 40°C
Hold time ‘1’ : 0°C/min
Rate temp : 10°C/min
Hold temp : 220°C
Hold Time ‘2’ : 5 min
Run time : 23 min
Gas flow : Constant velocity
Split : 1:20
Hydrogen : 45 mL/min
Zero Air : 450 mL/min
Condition for Head Space Sampler
Vial temperature : 100 °C
Needle temperature : 110 °C
Transfer line temperature : 120 °C
Injection volume : 0.06 mL
Thermostat : 15 min
High pressure inject : on
Head space mode : constant
Carrier gas pressure : 15 psi
Vial pressurization : 4 min
Withdraw time : 0.2 min
GC cycle time : 35 min
Solution preparation
Blank solution
Transfer 4.0 mL of Dimethyl sulphoxide in
headspace vial and seal it using vial crimper.
Standard stock solution
To a 100.0 mL volumetric flask containing 20.0
mL of Dimethyl sulphoxide, transfer about 250.0
mg of Isopropyl alcohol (IPA) dilute to volume
with Dimethyl sulphoxide and mix well.
Standard solution
Transfer 25.0 mL of standard stock solution into
100 mL volumetric flask, dilute to volume with
Dimethyl sulphoxide and mix.
Transfer 4.0 mL of the standard solution into a
head space vial, and seal it using vial crimper.](data:image/gif;base64,R0lGODlhAQABAIAAAAAAAP///yH5BAEAAAAALAAAAAABAAEAAAIBRAA7)