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This journal article describes three methods for determining two mixtures containing drotaverine hydrochloride: 1) HPLC separation and UV detection, 2) partial least squares chemometrics assisted spectrophotometry, and 3) principal component regression chemometrics assisted spectrophotometry. These methods were validated using internal validation, crossvalidation, and external validation on laboratory mixtures and pharmaceutical preparations. The results of the chemometrics methods agreed well with the HPLC method.
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This document describes a liquid chromatographic method for the simultaneous quantitative determination of candesartan cilexetil and hydrochlorothiazide in pharmaceutical dosage forms. A simple and sensitive RP-HPLC method was developed and validated. The method allows for the separation, identification and quantification of candesartan cilexetil and hydrochlorothiazide in tablet formulations using a C18 column with UV detection. The method was validated in terms of specificity, linearity, precision, accuracy and robustness.
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Pharmaceutical analysis & qc ii - SAM
This document discusses affinity chromatography, a separation method based on specific binding interactions between an immobilized ligand and its binding partner. It describes the three main steps of affinity purification: incubation to allow binding, washing away unbound components, and elution to recover the target molecule. Key aspects covered include the principle of molecular recognition and entrapment on the stationary phase, common chromatographic media like agarose beads, ligand selection and attachment, materials and procedures used, and applications in protein purification and studying drug interactions. Both advantages like high specificity and disadvantages like cost and limited lifetime are noted.
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Kinetic spectrophotometric determination of V(IV) in the presence of V(V) by ...
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This document describes a kinetic spectrophotometric method using the H-point standard addition method (HPSAM) to simultaneously determine vanadium(IV) and vanadium(V) or selectively determine vanadium(IV) in the presence of vanadium(V). The method utilizes the difference in rate of complex formation between vanadium(IV) and vanadium(V) with xylenol orange under acidic conditions. Vanadium(IV) can be determined in the range of 0.2-5 μg/ml with accuracy and precision, even in the presence of excess vanadium(V) and other metal ions. The method was successfully applied to synthetic mixtures and real samples to simultaneously or selectively determine vanadium(IVIntroduction to analytical chemistry
Analytical chemistry has been important since the early days of chemistry and provides methods to determine what elements and chemicals are present in a sample. Traditional techniques like qualitative analysis to determine presence/absence of compounds and quantitative analysis methods like gravimetric analysis and titration, along with modern instrumental techniques like spectroscopy, mass spectrometry, and chromatography, form the foundation of analytical chemistry. New hybrid techniques that combine multiple analytical methods are also increasingly used.
Indirect Simultaneous Kinetic Determination of Semicarbazide and Hydrazine in...
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This document describes a method using the H-point standard addition method (HPSAM) for the simultaneous determination of semicarbazide and hydrazine. The method is based on the reduction of Cu2+ to Cu+ by semicarbazide and hydrazine in the presence of neocuproine, followed by complex formation between Cu+ and neocuproine, producing a colored complex. The difference in the rates of reduction allows for the simultaneous analysis of both analytes. The method was able to determine semicarbazide in the range of 0.5-3.75 mg/ml and hydrazine in the range of 0.5-5 mg/ml in synthetic mixtures with differentAcamprosate Analytical
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- ACM is a drug used to treat alcohol dependence. Previous methods for quantifying ACM required complex extraction/derivatization steps.
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Simultaneous estimation of meclizine and nicotinic acid by using RP-HPLC
This document describes the development and validation of a reverse phase high performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of Meclizine and Nicotinic acid. The method utilizes a mobile phase of acetonitrile and potassium dihydrogen phosphate buffer with a flow rate of 1.0 mL/min. The retention times were 3.01 minutes for Meclizine and 6.07 minutes for Nicotinic acid. The method was validated and found to be accurate, precise, specific, linear, robust, sensitive and able to quantify the drugs in tablet dosage forms without interference from other components.
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Meu primeiro artigo internacional
This document presents a method for determining levels of psoralens like psoralen and bergapten in oral solutions of herbal medicines using liquid chromatography. The method involves extracting samples with chloroform, dissolving residues in methanol, and analyzing by HPLC. The method was validated in terms of linearity, accuracy, precision and specificity. Psoralen and bergapten were found to be stable in samples and solutions under various storage conditions. The method provides a fast and reliable means of quantifying psoralen levels in herbal medicines.
SIMULTANEOUS QUANTIFICATION OF TELMISARTAN AND METOPROLOL SUCCINATE IN TABLET...
The document describes the development and validation of a liquid chromatographic method for the simultaneous quantification of telmisartan and metoprolol succinate in tablets. The method utilizes a Nucleosil C18 column with a mobile phase of acetonitrile and potassium di-hydrogen orthophosphate buffer (pH 2.8) in a 60:40 ratio at a flow rate of 0.8mL/min. Telmisartan and metoprolol succinate were detected at 220nm with retention times of 3.392 and 5.221 minutes respectively. The method was validated and found to be accurate, precise and robust for the simultaneous analysis of both drugs in tablet formulations.
ANALYTICAL METHOD DEVELOPMENT AND VALIDATION HPLC UV
The document describes the development and validation of a reverse phase high performance liquid chromatography (RP-HPLC) method for the estimation of drugs in bulk and pharmaceutical dosage forms. It discusses the need for analytical methods in pharmaceutical analysis and introduces RP-HPLC as a commonly used technique. The document provides details of various studies done to develop and validate RP-HPLC methods for estimating specific drugs and drug combinations in research papers. It also provides chemical and pharmacological profiles of drugs that were estimated using RP-HPLC methods discussed in the literature review section. The aim is to develop a validated RP-HPLC method for estimation of a drug in bulk and marketed dosage form.
Meu segundo artigo internacional
This document describes a method for quantitatively analyzing three furanocoumarins (psoralen, bergapten, and 5-[3-(4,5-dihydro-5,5-dimethyl-4-oxo-2-furanyl)-butoxy]-7H-furo[3-2-g][1]benzopyran-7-one) in capsules and tablets using high-performance liquid chromatography with UV detection (HPLC-UV). The method was validated based on its linearity, accuracy, precision, and recovery. The analytical method provides a validated procedure for quantitatively analyzing these furanocoumarins in phytomedicinal capsules and tablets.
Art%3 a10.1007%2fs12161 013-9618-4
This document describes a new approach for fingerprint analysis of Chrysanthemum morifolium Ramat combining ultra-performance liquid chromatography (UPLC) and chemometrics methods. UPLC allowed for chromatographic separation and detection of components in 10 minutes, much faster than conventional HPLC methods. Good precision, reproducibility, and accuracy were obtained for six typical components. Consistent results were seen based on cultivation source. The method provides a more rapid quality control technique for C. morifolium Ramat.
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The aim of the present work was to develop a isocratict RP-HPLC for simultaneous analysis of ritonavir and lopinavir in tablet dosage form. Method: chromatographic system was optimized using a Agilent XDB C18(150 x 4.6mm,5µm) column with potassium dihydrogen phosphate (pH 4.6) and acetonitrile in the ratio of 45;55, as a mobile phase, at a flow rate of 1.0 ml/min. detection was carried out at 215nm by a photodiode array detector. Result: ritonavir and lopinavir were eluted with retention times of 4.821 and 3.814mins respectively. Beer’s lambert’s law was obeyed over the concentration ranges of 12.5 to 50µg/ml and 50 to 200µg/ml for ritonavir and lopinavir, respectively. Conclusion: the high recovery and low coefficients of variation confirm the suitability of the method for simultaneous analysis of both drugs in a tablet dosage form. Statistical analysis proves that the method is sensitive and significant for the analysis of ritonavir and lopinavir in pure and in pharmaceutical dosage form without any interference from the excipients. The method was validated in accordance with ICH guidelines. Validation revealed the method is specific, rapid, accurate, precise, reliable, and reproducible.
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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 injectionsMethod development and validation for the simultaneous estimation of sitaglip...
Method development and validation for the simultaneous estimation of sitagliptin and metformin in tablet dosage form by RP-HPLC
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My final presentation
This document summarizes a dissertation submitted for a PharmD degree. It describes the development and validation of an analytical method for the quantitative analysis of metoclopramide hydrochloride using HPLC and UV spectroscopy. The objectives are to develop a simple, sensitive, accurate and economic RP-HPLC method and validate it according to ICH guidelines. A literature review provided background on previous related studies and informed the methodology. The method was developed using an HPLC system with a C8 column, gradient elution and UV detection. The method will be validated for accuracy, precision and other parameters and applied to analyze metoclopramide in samples.
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Development and Validation of RP-HPLC method for the simultaneous estimation of Miglitol and Metformin Hcl in Pharmaceutical formulations
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This document describes the development and validation of a reverse-phase high-performance liquid chromatography (RP-HPLC) method for the quantitative analysis of daclatasvir in pharmaceutical formulations. The method utilizes a C18 column, mobile phase of acetonitrile and 0.1% formic acid buffer at a ratio of 40:60, and detection wavelength of 305 nm. Standard and sample solutions of daclatasvir were prepared and analyzed using the optimized method. The results demonstrate that the developed RP-HPLC method is accurate, precise, sensitive and stability-indicating for the analysis of daclatasvir in pharmaceutical dosage forms.Application of chromatography in pharmaceutics
Chromatography is a separation technique used in pharmaceutical analysis. It works by separating components in a mixture as they move through stationary and mobile phases at different rates. High performance liquid chromatography (HPLC) is commonly used, accounting for about 50% of separations. Chromatography is applied in pharmaceutical analysis for stability studies, bulk analysis, tablet analysis, and pharmacokinetic studies. It can be used to monitor drug and degradation levels over time under various conditions to ensure stability. Several examples are provided of developing and validating HPLC methods for analyzing specific drugs in bulk and formulations. References are also included.
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Stability indicating method development and validation for the estimation of Doxorubicin by using RP-HPLC method in a bulk and pharmaceutical dosage form
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Major process related unknown impurity associated with the synthesis of Hydralazine hydrochloride bulk drug was detected by high performance liquid chromatography (HPLC) and was subjected to high resolution accurate liquid chromatography mass spectroscopy (HR/AM-LCMS) for identification. The proposed impurity was isolated from Hydralazine hydrochloride active pharmaceutical ingredient (API) by preparative chromatographic method and was injected on HPLC for comparison of retention time with that of the unknown process related impurity in Hydralazine hydrochloride. The molecular ion peak of preparatively isolated impurity and that of unknown process related impurity in Hydralazine hydrochloride were compared for confirmation. The postulated structure was unambiguously confirmed with the help of HR/AM- LC MS/MS, NMR and FTIR data proposed to be 1-(2-phthalazin-1-ylhydrazino)phthalazine (Hazh Dimer). This impurity of Hydralazine hydrochloride is not been previously reported. A rapid Acquity H-class gradient method with runtime of 15.0min was developed for Quantitation on Unisphere Cyno column and validated for parameters such as accuracy, precision, linearity and range, robustness. The LOD and LOQ of method were 0081% and 0.0246% respectively.
HPLC and its relation with mass spectroscopy
This document describes a PowerPoint presentation on HPLC and its relationship to mass spectrometry. The presentation was created by a group of students for their 4th semester course. It introduces HPLC and how it separates mixtures based on interactions with stationary and mobile phases. It then explains how HPLC can be combined with mass spectrometry (LC-MS) to further analyze separated compounds. The presentation covers operating principles, applications in fields like forensics and pharmaceuticals, examples of research using the techniques, and concludes that LC-MS is widely used for qualitative and quantitative analysis in various industries and research.
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This document describes the development and validation of a quantitative method for determining penbutolol and its metabolite 4-hydroxy penbutolol in human plasma using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method involves solid phase extraction of the analytes from plasma followed by separation using liquid chromatography with mass spectrometric detection in multiple reaction monitoring mode. The method was validated according to FDA guidelines and showed good linearity, accuracy, precision, recovery, selectivity and stability. The developed and validated LC-MS/MS method was found to be suitable for pharmacokinetic studies of penbutolol in human volunteers.
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Aplicacion calibracion
- 1. Journal Article El-Gindy,A.; Emara,S.; Shaaban,H. Título Validation and application of chemometrics-assisted spectrophotometry and liquid chromatography for simultaneous determination of two ternary mixtures containing drotaverine hydrochloride Publicación Completa Journal of AOAC International Publicación Abreviada J.AOAC Int. Año de Publicación 2010 Volumen 93 Ejemplar 2 Página Inicial 536 Otras Páginas 548 Resumen Three methods were developed for the determination of two ternary mixtures containing drotaverine hydrochloride (DR) with caffeine and paracetamol (mixture 1) and DR with metronidazole and diloxanide furoate (mixture 2). The first method depends on HPLC separation on an RP C18 column at ambient temperature with the mobile phase methanol-water, pH 3.1 (50 + 50, v/v) and UV detection at 213 nm for mixture 1, and the mobile phase acetonitrile-25 mM potassium dihydrogen phosphate, pH 4.6 (55 + 45, v/v) with UV detection at 235 nm for mixture 2. The other two chemometric methods applied were partial least squares (PLS-1) and principal component regression (PCR). These approaches were successfully applied to quantify the five drugs in two ternary mixtures using information included in the UV absorption spectra of appropriate solutions in the wavelength range of 210-300 nm with 1 nm intervals. Calibration of PCR and PLS-1 models was evaluated by internal validation (prediction of compounds in its own designed training set of calibration), by crossvalidation (obtaining statistical parameters that show the efficiency for a calibration fit model), and by external validation (using laboratory-prepared mixtures and pharmaceutical preparations). The proposed methods were successfully applied for the determination of the two ternary combinations in laboratory-prepared mixtures and commercial tablets; the results of PLS-1 and PCR methods were compared with the HPLC method, and a good agreement was found. Dirección/Afiliación del Autor Affiliation: Suez Canal University, Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Ismailia 41522, Egypt Base de Datos SCOPUS Fuente de Datos Scopus Fecha Recuperada 6 June 2012
- 2. Creado 6/6/2012 11:20:43 Zona horaria local (GMT +1hr) Ultima Modificación 6/6/2012 11:26:26 Zona horaria local (GMT +1hr) URL http://www.scopus.com/inward/record.url?eid=2-s2.0- 77952755707&partnerID=40&md5=bb6eb60a7c185c2cad52224c3be9f071