A Validated Method for the Quality Control of Andrographis paniculata Preparations

Planta Medica ◽  
2017 ◽  
Vol 83 (14/15) ◽  
pp. 1207-1213 ◽  
Author(s):  
Anastasia Karioti ◽  
Patricia Timoteo ◽  
Maria Bergonzi ◽  
Anna Bilia
Keyword(s):  
Quality Control ◽  
Time Course ◽  
Symptomatic Treatment ◽  
Reversed Phase ◽  
Andrographis Paniculata ◽  
Gradient System ◽  
Solvent Mixtures ◽  
Relative Standard ◽  
Precision And Accuracy

Abstract Andrographis paniculata is a herbal drug of Asian traditional medicine largely employed for the treatment of several diseases. Recently, it has been introduced in Europe for the prophylactic and symptomatic treatment of common cold and as an ingredient of dietary supplements. The active principles are diterpenes with andrographolide as the main representative. In the present study, an analytical protocol was developed for the determination of the main constituents in the herb and preparations of A. paniculata. Three different extraction protocols (methanol extraction using a modified Soxhlet procedure, maceration under ultrasonication, and decoction) were tested. Ultrasonication achieved the highest content of analytes. HPLC conditions were optimized in terms of solvent mixtures, time course, and temperature. A reversed phase C18 column eluted with a gradient system consisting of acetonitrile and acidified water and including an isocratic step at 30 °C was used. The HPLC method was validated for linearity, limits of quantitation and detection, repeatability, precision, and accuracy. The overall method was validated for precision and accuracy over at least three different concentration levels. Relative standard deviation was less than 1.13%, whereas recovery was between 95.50% and 97.19%. The method also proved to be suitable for the determination of a large number of commercial samples and was proposed to the European Pharmacopoeia for the quality control of Andrographidis herba.

UV spectroscopic method for determination of phenytoin in bulk and injection forms

2019 ◽  
Author(s):  
Chem Int
Keyword(s):  
Quality Control ◽  
Spectrophotometric Method ◽  
Spectroscopic Method ◽  
Ich Guidelines ◽  
Precision And Accuracy ◽  
Routine Quality Control

Recent study was conducted to develop a simple UV spectrophotometric method to determine Phenytoin in bulk and injection form according to official requirement and validate as per ICH guidelines. λmax of Phenytoin was found 202 nm. Linearity existed perceived in the concentration assortment 2-8 μg/ml (r2 = 0.999) for the method. The method was validated pertaining to linearity, precision and accuracy studies, LOD and LOQ consistent with ICH guidelines. The existent method was establish to be simple, linear, precise, accurate as well as sensitive and can be applied for routine quality control enquiry for the analysis of Phenytoin in bulk and injection form.

scholarly journals Simultaneous determination of clobutinol hydrochloride and doxylamine succinate from syrups by RP HPLC using a new stationary phase containing embedded urea polar groups

2012 ◽  
Vol 48 (2) ◽  
pp. 315-323 ◽  
Author(s):  
Paulo Cesar Pires Rosa ◽  
Isabel Cristina Sales Fontes Jardim
Keyword(s):  
Stationary Phase ◽  
Simultaneous Determination ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Polar Groups ◽  
Ich Guidelines ◽  
Relative Standard ◽  
New Stationary Phase

A new, simple, fast, reproducible and sensitive reversed phase HPLC method, using a new stationary phase containing embedded urea polar groups, has been developed and validated for the simultaneous determination of clobutinol hydrochloride (CLO) and doxylamine succinate (DOX) in syrups. The determination was carried out on a C8 urea column (125 mm x 3.9 mm i.d., 5 µm particle size) synthetized at the Liquid Chomatography Laboratory (LabCrom) of the Chemistry Institute of Unicamp. The mobile phase consisted of a mixture of acetonitrile:methanol:phosphate buffer (pH 2.5) in the gradient mode. The diode array detector (DAD) was operated at 230 nm for CLO and 262 nm for DOX. The method showed adequate precision, with relative standard deviations (RSD) less than 1%. The presence of the excipients did not interfere in the results of the analysis. Accuracy was determined by adding standards of the drugs to a placebo and good recovery values were obtained. The analytical curves were linear (r² 0.9999 for CLO and 0.9998 for DOX) over a wide concentration range (2.4-336 µg mL-1 for CLO and 2.3-63 µg mL-1 for DOX). The solutions were stable for at least 72 hours at room temperature. The criteria for validation using the ICH guidelines were fulfilled.

scholarly journals Application of Liquid Chromatography to the Simultaneous Determination of Acetylsalicylic Acid, Caffeine, Codeine, Paracetamol, Pyridoxine, and Thiamine in Pharmaceutical Preparations

2001 ◽  
Vol 84 (3) ◽  
pp. 676-683 ◽  
Author(s):  
Natividad Ramos-Martos ◽  
Francisco Aguirre-Gómez ◽  
Antonio Molina-Díaz ◽  
Luis F Capitán-Vallvey
Keyword(s):  
Salicylic Acid ◽  
Acetylsalicylic Acid ◽  
Simultaneous Determination ◽  
Pharmaceutical Preparations ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract This paper describes a rapid reversed-phase liquid chromatographic method, with UV detection, for the simultaneous determination of acetylsalicylic acid, caffeine, codeine, paracetamol, pyridoxine, and thiamine in pharmaceutical preparations. A reversed-phase C18 Nucleosil column is used. The mobile phase consists of 2 successive eluants: water (5 min) and acetonitrile–water (75 + 25, v/v; 9 min), both adjusted to pH 2.1 with phosphoric acid. Before determination acetylsalicylic acid is completely converted to salicylic acid by alkaline hydrolysis. Salicylic acid, caffeine, paracetamol, pyridoxine, and thiamine are all detected at 285 nm, whereas codeine is detected at 240 nm. Calibration curves were linear for salicylic acid, caffeine, paracetamol, and pyridoxine in the range of 50–500 mg/L, and for codeine and thiamine in the range of 50–1000 mg/L. The method was applied to the analysis of 13 fortified commercial pharmaceutical preparations. Recoveries ranged from 92.6 to 105.5%, with relative standard deviations of 1.1–5.8%.

scholarly journals Development and validation of reversed phase high performance liquid chromatography (RP-HPLC) for quantification of captopril in rabbit plasma

2020 ◽  
Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Rabbit Plasma ◽  
Rp Hplc ◽  
Relative Standard

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.

scholarly journals Fast and selective HPLC-DAD method for determination of pholcodine and related substances

2011 ◽  
Vol 30 (2) ◽  
pp. 139 ◽  
Author(s):  
Ana Petkovska ◽  
Hristina Babunovska ◽  
Marina Stefova
Keyword(s):  
Quality Control ◽  
Degradation Products ◽  
Ammonium Hydroxide ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Real Sample Analysis ◽  
Related Substances ◽  
Structural Analogues ◽  
Reliable Methods

Quality control of pharmaceuticals requires development of fast, efficient and reliable methods for determination of active compounds as well as known and very often unknown impurities within defined concentration ranges. In this work, a simple and rapid HPLC-UV-DAD method for identification and quantification of pholcodine process related impurities and some degradation products was developed and validated. Pholcodine and its five structural analogues such as morphine, codeine, thebaine, oripavine, and papaverine were separated in less than 10 minutes using reversed phase LiChrospher C-8 column. For optimal chromatographic performance with reproducible retention times, gradient elution with 2% ammonium hydroxide in water and acetonitrile was used. The method was validated by establishing its selectivity, specifity, sensitivity, linearity, intra- and inter-day precision and robustness. All tested parameters confirmed that the method is suitable for determination of pholcodine and its five impurities in pharmaceutical drug samples. The results obtained from real sample analysis give support to the suitability of the proposed method for the purpose of quality control.

scholarly journals Development of a New High-Performance Liquid Chromatographic Method for the Determination of Ceftazidime

2008 ◽  
Vol 91 (4) ◽  
pp. 739-743 ◽  
Author(s):  
Andréia de Haro Moreno ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Calibration Graph ◽  
Raw Material ◽  
Relative Standard ◽  
Validation Parameters ◽  
Liquid Chromatographic

Abstract A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of ceftazidime in pharmaceuticals. The method validation parameters yielded good results and included range, linearity, precision, accuracy, specificity, and recovery. The excipients in the commercial powder for injection did not interfere with the assay. Reversed-phase chromatography was used for the HPLC separation on a Waters C18 (WAT 054275; Milford, MA) column with methanolwater (70 + 30, v/v) as the mobile phase pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 245 nm. The calibration graph for ceftazidime was linear from 50.0 to 300.0 g/mL. The values for interday and intraday precision (relative standard deviation) were <1. The results obtained by the HPLC method were calculated statistically by analysis of variance. We concluded that the HPLC method is satisfactory for the determination of ceftazidime in the raw material and pharmaceuticals.

scholarly journals Identification of Allantoin, Uric Acid, and Indoxyl Sulfate as Biochemical Indicators of Filth in Food Packaging by LC

2001 ◽  
Vol 84 (3) ◽  
pp. 782-788 ◽  
Author(s):  
Marvin Carlson ◽  
Richard D Thompson
Keyword(s):  
Uric Acid ◽  
Food Packaging ◽  
Reversed Phase ◽  
Indoxyl Sulfate ◽  
Rat Urine ◽  
Relative Standard ◽  
Analyte Content ◽  
Corrugated Cardboard ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method was developed for the determination of allantoin, uric acid, and indoxyl sulfate in mammalian urine contaminated packaging material including paper bagging, corrugated cardboard, grayboard, and burlap bagging. The procedure involves solvent extraction and isolation of the 3 analytes by reversed-phase LC with ultraviolet detection at 225 nm for allantoin and 286 nm for uric acid and indoxyl sulfate. The composition of authentic mammalian urine such as mouse, rat, cat, dog, and human were also determined with regard to the 3 compounds of interest. A linear concentration range of 0.11–20.4, 0.02–10.0, and 0.04–30.0 μg/mL was obtained for allantoin, uric acid, and indoxyl sulfate, respectively. Limits of detection (LOD) and quantitation (LOQ) were 0.0104 and 0.0345 μg/mL for allantoin; 0.0018 and 0.0060 μg/mL for uric acid; and 0.0049 and 0.0165 μg/mL for indoxyl sulfate, respectively. Interday relative standard deviation values for a mixture of standard allantoin, uric acid, and indoxyl sulfate (n = 5) were 0.97, 0.80, and 0.94%, respectively. Analyte composition for 5 types of authentic mammalian urine varied from 0.19–6.88 mg/mL allantoin; 0.08–0.57 mg/mL uric acid; and 0.03–0.78 mg/mL indoxyl sulfate. Analyte content for 8 samples including 2 samples each for paper, cardboard, grayboard, and burlap bagging each contaminated with mouse or rat urine ranged from <LOD to 4598 μg/gm allantoin; <LOD to 202 μg/gm uric acid; and 17.5 to 616 μg/gm indoxyl sulfate. Recoveries of allantoin, uric acid, and indoxyl sulfate from 11 fortified samples (4 types) for both mouse and rat urine ranged from 28.2 to 114.1% for allantoin; 32.6 to 123.4% for uric acid; and 52.6 to 118.2% for indoxyl sulfate.

scholarly journals Supramolecular Solvent-Based Liquid Phase Microextraction Combined with Ion-Pairing Reversed-Phase HPLC for the Determination of Quats in Vegetable Samples

Toxics ◽  
2019 ◽  
Vol 7 (4) ◽  
pp. 60
Author(s):  
Sophon Hem ◽  
Netsirin Gissawong ◽  
Supalax Srijaranai ◽  
Suthasinee Boonchiangma
Keyword(s):  
Liquid Phase ◽  
Sodium Dodecyl ◽  
Tetrabutylammonium Bromide ◽  
Ion Pairing ◽  
Reversed Phase ◽  
Liquid Phase Microextraction ◽  
Vegetable Samples ◽  
Relative Standard ◽  
Supramolecular Solvent

In this study, we used anion supramolecular solvent (SUPRAS) prepared from a mixture of an anionic surfactant, sodium dodecyl sulfate (SDS), and a cationic surfactant, tetrabutylammonium bromide (TBABr), as the extraction solvent in liquid phase microextraction (LPME) of paraquat (PQ) and diquat (DQ). The enriched PQ and DQ in the SUPRAS phase were simultaneously analyzed by ion-pairing reversed-phase high performance liquid chromatography. PQ and DQ were successfully extracted by LPME via electrostatic interaction between the positive charge of the quats and the negative charge of SUPRAS. PQ, DQ, and ethyl viologen (the internal standard) were separated within 15 min on a C18 column, with the mobile phase containing 1-dodecanesulfonic acid and triethylamine, via UV detection. The optimized conditions for the extraction of 10 mL aqueous solution are 50 μL of SUPRAS prepared from a mixture of SDS and TBABr at a mole ratio of 1:0.5, vortexed for 10 s at 1800 rpm, and centrifugation for 1 min at 3500 rpm. The obtained enrichment factors were 22 and 26 with limits of detection of 1.5 and 2.8 µg L−1 for DQ and PQ, respectively. The precision was good with relative standard deviations less than 3.86%. The proposed method was successfully applied for the determination of PQ and DQ in vegetable samples and recoveries were found in the range of 75.0% to 106.7%.

scholarly journals Simultaneous Determination of Chlorpheniramine Maleate and Dexamethasone in a Tablet Dosage Form by Liquid Chromatography

2005 ◽  
Vol 88 (6) ◽  
pp. 1677-1683 ◽  
Author(s):  
María A Moyano ◽  
María A Rosasco ◽  
María T Pizzorno ◽  
Adriana I Segall
Keyword(s):  
Potassium Phosphate ◽  
Reversed Phase ◽  
Chlorpheniramine Maleate ◽  
Constant Flow Rate ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Tablet Dosage ◽  
Liquid Chromatographic ◽  
Interday Precision

Abstract An accurate, simple, reproducible, and sensible liquid chromatographic method was developed and validated for the determination of chlorpheniramine maleate and dexamethasone in a tablet formulation. The analysis was performed at room temperature on a reversed-phase C18 column with UV detection at 254 nm. The mobile phase consisted of 7.5 mM monobasic potassium phosphate in methanol–water (62.5 + 37.5) at a constant flow rate of 1 mL/min. The method was validated in terms of linearity, precision, accuracy, and specificity by forced decomposition of chlorpheniramine maleate and dexamethasone initiated by using acid, base, water, hydrogen peroxide, heat, and light. The response was linear in the ranges of 0.04–0.12 and 0.006–0.016 mg/mL for chlorpheniramine maleate (r2 = 0.9999) and dexamethasone (r2 = 0.9994), respectively. The relative standard deviation values for intra- and interday precision studies were 2.39 and 2.02, respectively, for chlorpheniramine maleate and 2.39 and 1.25, respectively, for dexamethasone. Recoveries ranged from 95.07 to 101.95% for chlorpheniramine maleate and from 97.75 to 102.10% for dexamethasone.

scholarly journals Simultaneous Determination of Bioactive Xanthone Glycosides and Norlignans from Ethanolic Extract of Anemarrhena asphodeloides by Liquid Chromatography

2008 ◽  
Vol 91 (6) ◽  
pp. 1271-1277 ◽  
Author(s):  
M Nurul Islam ◽  
Hye Hyun Yoo ◽  
Jun Lee ◽  
Joo Won Nam ◽  
Eun Kyoung Seo ◽  
...  
Keyword(s):  
Ethanolic Extract ◽  
Reversed Phase ◽  
Linear Behavior ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Aggregation Inhibition ◽  
Phase Liquid ◽  
Liquid Chromatographic ◽  
Anemarrhena Asphodeloides

Abstract The rhizomes of Anemarrhena asphodeloides Bunge (Liliaceae) are prescribed as crude drugs in herbal medication for the treatment of various diseases such as diabetes, inflammation, and platelet aggregation inhibition. A simple, sensitive, and precise reversed-phase liquid chromatographic method was developed to study the quantitative determination of 5 bioactive compounds from these rhizomes, namely, neomangiferin, mangiferin, isomangiferin, nyasol, and methylnyasol. Chromatographic analysis was performed on Capcell Pak C18 column (150 4.6 mm, 3 m) with a mobile phase consisting of acetonitrile, methanol, and 0.1 formic acid at a flow rate of 1.00 mL/min. Quantitation was performed using a UV-visible detector at 260 nm. The method for the determination of reported medicinal agents was accurate and reproducible. Excellent linear behavior was observed over the investigated concentration range of 2.5100.0 g/mL for neomangiferin; 1.560.0 g/mL for mangiferin; 0.520.0 g/mL for nyasol; and 0.220.0 g/mL for methylnyasol; correlation coefficient >0.99. The intraday and interday precision over the concentration range of compounds was <6.6 (relative standard deviation) and accuracy was between 94.9 and 109.3. This method can be successfully applied for the analysis of medicinal compounds from the ethanolic extract of A. asphodeloides Bunge.

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