Development and Validation of Analytical Method for Simultaneous Estimation of Active Constituents in a Polyherbal Ointment by Gas Chromatography

2019 ◽  
Vol 102 (4) ◽  
pp. 1027-1032
Author(s):  
Vishal R Patel ◽  
Hardik K Soni ◽  
Vikram B Trivedi ◽  
Jigna B Patel ◽  
Suresh Jain
Keyword(s):  
Methyl Salicylate ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Simultaneous Estimation ◽  
Internal Standard Method ◽  
Active Constituents ◽  
Flame Ionization ◽  
Quality Control Testing ◽  
Marker Compounds ◽  
Development And Validation

Abstract Background: The simultaneous, quantitative determination of all active ingredients present in the analgesic formulation (Dazzle ointment) requires an ideal and novel method by which these phytoconstituents can be separated with the highest resolution without any interference from one another. Objective: The present work was conducted to develop and validate a quantitative method for the simultaneous estimation of all five phytoconstituents present in a polyherbal analgesic ointment by GC. Methods: α-Pinene, 1,8-cineole, camphor, menthol, and methyl salicylate present in the ingredients of the ointment were analyzed and quantified by GC using a crosslinked 5% phenyl polydimethylsiloxane capillary column, nitrogen as a carrier gas, and a flame-ionization detector. Aniline was used as the internal standard. Method validation was also performed in order to demonstrate its selectivity, linearity, accuracy, precision, LOD, LOQ, and robustness. Results: The calibration curves of all five marker compounds showed good linear correlation coefficients (r2 >0.998) within the tested ranges. The precision of the method was tested by carrying out intra- and interday analyses of the same sample. RSD values were observed to be <1.00%. The accuracy of the method, determined by performing recovery studies, was found to be between 99.25 and 101.39%. The developed method was also demonstrated to be robust (RSD <1.29%) by making small but deliberate variations in method parameters. Conclusions: The developed GC method is simple, precise, and accurate, it and can be used for the rapid quality control testing of the polyherbal formulation. Highlights: The developed GC method will assist in the standardization of polyherbal analgesic formulation consists of α-pinene, 1,8-cineole, camphor, menthol, and methyl salicylate as active constituents.

ANALYTICAL METHOD DEVELOPMENT AND ITS VALIDATION FOR EVALUATION OF POLYHERBAL FORMULATION

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (10) ◽  
pp. 66-68
Author(s):  
◽  
A. P Jadhav
Keyword(s):  
Immune Response ◽  
Ethyl Acetate ◽  
Analytical Method ◽  
Mobile Phase ◽  
Method Development ◽  
Simultaneous Estimation ◽  
Active Constituents ◽  
Polyherbal Formulation ◽  
Marker Compounds ◽  
Hptlc Method

Talekt capsule is a branded polyherbal formulation used for enhancing the immune response to dermal infections and also for treating skin disorders. Curcumin and embelin, which are the active constituents of Haridra and Vidanga, respectively were used as marker compounds for developing a simple, accurate, precise and robust HPTLC method for simultaneous estimation. The mobile phase of toluene: ethyl acetate: formic acid (6.5: 3: 0.2 v/v/v) was used for separation. 381nm was used as wavelength for analysis. The Rf value obtained for curcumin, and embelin was found to be 0.51 ± 0.2 and 0.33 ± 0.2, respectively. The developed method was validated on the basis of ICH Q2 (R1) guidelines.

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF ABACAVIR SULPHATE AND LAMIVUDINE IN TABLET DOSAGE FORM BY RP-HPLC

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (08) ◽  
pp. 12-16
Author(s):  
S Vidyadhara ◽  
◽  
L. S Reddyvalam ◽  
T. Koduri ◽  
P. K. Borra ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Correlation Coefficients ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple, accurate, precise high-performance liquid chromatographic (HPLC) method has been developed and validated for the simultaneous determination of abacavir sulphate (ABA) and lamivudine (LAM) in combined dosage form. Separation was performed on a C18 column [Agilent ODS UG 5 column, 250 mm x 4.5 mm], with methanol: water (50:50 V/V) isocratic elution using a flow rate of 1mL/min. Good sensitivity was observed with UV detection at 277 nm. After method development, the interference of other active compounds and excipients, repeatability and linearity, were investigated. Retention times of LAM and ABA were found to be 3.3 and 6.3 min, respectively. The method was validated over the range from 2.5-12.5 μg/mL for LAM and 5-25 μg/mL for ABA with correlation coefficients of 0.9997 and 0.9996, respectively. This method was shown to be accurate, robust, selective, linear, and repeatable and can be successfully employed in routine quality control for the simultaneous analysis of ABA and LAM in tablets.

scholarly journals DEVELOPMENT AND VALIDATION OF LIQUID CHROMATOGRAPHY COUPLED WITH TANDEM MASS SPECTROMETRY METHOD FOR ESTIMATION OF LENVATINIB IN HUMAN PLASMA

2017 ◽  
Vol 10 (7) ◽  
pp. 120
Author(s):  
Srikanth I ◽  
Prameela Rani A
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Tandem Mass ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Mode ◽  
Development And Validation

Objective: This study was to develop and validate a liquid chromatography–tandem mass spectrometry (LC–MS/MS) for the quantification of lenvatinib (LT) in human plasma.Methods: A simple, sensitive and specific LC–MS/MS method was developed for quantification of LT in human plasma using LTD4 as internal standard (IS). The analytical method consists of liquid–liquid extraction of plasma sample followed by the determination of LT by a LC–MS/MS. The analyte was separated on a Zorbax Eclipse XDB-C18 (150×4.6 mm, 5 μ) column with an isocratic mobile phase of acetontrile:0.1% formic acid (80:20 v/v) at a flow rate of 0.6 mL/minutes. The protonated ions were formed by a turbolon spray in a positive mode were used to detect analyte and IS. The MS/MS detection was made by monitoring the fragmentation of m/z 427.10→370.10 for LT and m/z 430.30→370.10 for IS on a MS.Result: The method was validated with the correlation coefficients of (r2) ≥0.995 over a linear concentration range of 10.20-501.60 pg/mL. This method demonstrated intra- and inter-day precision within 1.06-2.42% and 0.03-0.55% and accuracy within 95.64-100.08% and 97.16-100.07%.Conclusion: This method is suitable and convenient to pharmacokinetics and bioavailability studies for estimation of LT in biological samples by LC–MS/MS.

scholarly journals Validation of an HPLC method for the simultaneous determination of eletriptan and UK 120.413

2006 ◽  
Vol 71 (11) ◽  
pp. 1195-1205 ◽  
Author(s):  
Mira Zecevic ◽  
Biljana Jocic ◽  
Snezana Agatonovic-Kustrin ◽  
Ljiljana Zivanovic
Keyword(s):  
Mobile Phase ◽  
Analytical Procedure ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Control Analysis ◽  
Internal Standard Method ◽  
Rp Hplc ◽  
Good Repeatability

Arapid and sensitive RPHPLCmethod was developed for the routine control analysis of eletriptan hydrobromide and its organic impurity UK 120.413 in Relpax? tablets. The chromatography was performed at 20?C using a C18 XTerra ? (5 ?m, 150 x 4,6 mm) column at a flow rate 1.0 ml/min. The drug and its impurity were detected at 225 nm. The mobile phase consisted of TEA (1 %) - methanol (67.2:32.8 v/v), the pH of which was adjusted to 6.8 with 85 % orthophosphoric acid. Quantification was accomplished by the internal standard method. The developed RP HPLC method was validated by testing: accuracy, precision, repeatability, specificity, detection limit, quantification limit, linearity, robustness and sensitivity. High linearity of the analytical procedure was confirmed over the concentration range of 0.05 - 1.00 mg/ml for eletriptan hydrobromide and from 0.10 - 1.50 ?g/ml for UK 120.413, with correlation coefficients greater than r = 0.995. The low value of the RSD expressed the good repeatability and precision of the method. Experimental design and a response surface method were used to test robustness of the analytical procedure and to evaluate the effect of variation of the method parameters, namely the mobile phase composition, pH and temperature. They showed small deviations from the method setting. The good recovery and low RSD confirm the suitability of the proposed RP HPLC method for the routine determination of eletriptan hydrobromide and its impurity UK 120.413 in Relpax? tables.

Development and Validation of a Rapid and Sensitive Method for the Simultaneous Estimation of Gemigliptin and Teneligliptin in Bulk and Dosage Forms by Using Liquid Chromatography-tandem Mass Spectrometry

2020 ◽  
Vol 16 (8) ◽  
pp. 1104-1111
Author(s):  
Amrish Chandra ◽  
Ramji Rathod ◽  
Faraat Ali ◽  
Anuj Prakash ◽  
Robin Kumar ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Internal Standard ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Simultaneous Estimation ◽  
Liquid Chromatography Tandem Mass ◽  
Sensitivity And Selectivity ◽  
Positive Mode ◽  
Development And Validation

Background: A simple and sensitive ultra-performance liquid chromatography-mass spectrometry method was developed and validated to measure the concentrations of gemigliptin (GEM) and teneligliptin (TEN) using pioglitazone (PIO) as an internal standard. Methods: Chromatographic separation of two gliptins was achieved on a C-18 (100 mm X 2.1 mm, 2.7 μm) column using a mobile phase consisting of formic acid in water (0.1 % v/ v): acetonitrile in gradient elution. Electrospray ionization (ESI) source was operated in positive mode (ionization). Targeted MS-MS mode on a quadrupole time of flight (Q-TOF) mass spectrometer was used to quantify the drugs utilizing the mass transitions of 490.1 (m/z), 427.2 (m/z) and 357.1 (m/z) for GEM, TEN and PIO, respectively. Results: As per ICH Q2R1 guidelines, a detailed validation of the method was carried out and the standard curves were found to be linear between the concentration ranges of 509.8-1529.4 ng mL-1 and 510.6-1531.7 ng mL-1 for GEM and TEN, respectively. Precision and accuracy results were found to be within the acceptable limits. The mean recovery was found to be 98.8± 0.76 % (GEM) and 98.6 ±0.98 % (TEN), respectively. Conclusions: The optimized validated UPLC-QTOF (MS-MS) method offered the advantage of shorter analytical times and higher sensitivity and selectivity to the nanogram level.

Simultaneous quantification of oxcarbazepine and its active metabolite in spiked human plasma using ultra performance liquid chromatography–MS/MS

Bioanalysis ◽  
2021 ◽  
Author(s):  
Karthik Rajendran ◽  
Bhadram Kalyan Chekraverthy ◽  
Rajendran Sankham Devendran ◽  
R Jasmin Sajini ◽  
Krishnaveni Nagappan
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Simultaneous Estimation ◽  
Internal Standard Method ◽  
Formulation Development ◽  
Chromatography Analysis ◽  
New Formulation

Aim: Clinical monitoring of oxcarbazepine (OXC) and its metabolite licarbazepine (MHD) in biological matrix requires a sensitive and validated analytical method. The aim of this study is to develop and validate an optimized ultra performance liquid chromatography–MS/MS based bioanalytical method for the simultaneous estimation of OXC and its metabolite MHD in human plasma, using deuterated internal standard method. Materials & methods: A reverse phase ultra performance liquid chromatography analysis and mass spectrometric detection was performed using electrospray ionization in positive ion mode as interface, multiple reaction monitoring as mode of acquisition. Results & conclusion: The linearity range was 10–4011 ng/ml for OXC and 40–16061 ng/ml for MHD. The kinetic parameters were calculated and compared for bioequivalence. This method fulfilled the validation guidelines, could be employed for determining bioavailability and in new formulation development studies.

RP-HPLC METHOD DEVELOPMENT AND ITS VALIDATION FOR EVALUATION OF POLYHERBAL FORMULATION

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (10) ◽  
pp. 68-70
Author(s):  
K. Sankar ◽  
◽  
A. P. Jadhav
Keyword(s):  
Immune Response ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Active Constituents ◽  
Polyherbal Formulation ◽  
Rp Hplc ◽  
Marker Compounds ◽  
Hplc Method Development

Curcumin and embelin, which are the active constituents of Haridra and Vidanga, respectively, were used as marker compounds for developing a simple, accurate, precise and robust RP-HPLC method for simultaneous estimation from Talekt capsule. It is a polyherbal formulation used for enhancing the immune response to dermal infections and also for treating skin disorders. The mobile phase of methanol: 1% ortho phosphoric acid in water in the ratio of 90:10 V/V was used for separation. Retention time of curcumin and embelin were found to be 2.77 ± 0.2 minutes and 7.77 ± 0.2 minutes, respectively. The developed method was validated as per ICH Q2 (R1) guidelines.

scholarly journals Development and Validation of LC Method for the Determination of Famciclovir in Pharmaceutical Formulation Using an Experimental Design

2008 ◽  
Vol 5 (1) ◽  
pp. 58-67 ◽  
Author(s):  
Srinivas Vishnumulaka ◽  
Narasimha Rao Medicherla ◽  
Allam Appa Rao ◽  
G. Edela Srinubabu
Keyword(s):  
Experimental Design ◽  
Flow Rate ◽  
Mobile Phase ◽  
Internal Standard ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Internal Standard Method ◽  
Intermediate Precision ◽  
Mobile Phase Flow Rate ◽  
Development And Validation

A rapid and sensitive RP-HPLC method with UV detection (242 nm) for routine analysis of famciclovir in pharmaceutical formulations was developed. Chromatography was performed with mobile phase containing a mixture of methanol and phosphate buffer (50:50,v/v) with flow rate 1.0 mL min−1. Quantitation was accomplished with internal standard method. The procedure was validated for linearity (correlation coefficient =0.9999), accuracy, robustness and intermediate precision. Experimental design was used for validation of robustness and intermediate precision. To test robustness, three factors were considered; percentage v/v of methanol in mobile phase, flow rate and pH; flow rate, the percentage of organic modifier and pH have considerable important effect on the response. For intermediate precision measure the variables considered were: analyst, equipment and number of days. The RSD value (0.86%,n=24) indicated an acceptable precision of the analytical method. The proposed method was simple, sensitive, precise, accurate and quick and useful for routine quality control.

scholarly journals Analytical method development and validation for simultaneous estimation of monoammonium glycyrrhizinate and sennoside-B in polyherbal laxative tablet using RP-HPLC

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Madhavi Patel ◽  
Shivangi Chauhan ◽  
Vishal Patel ◽  
Hardik Soni ◽  
Vikram Trivedi
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Correlation Coefficients ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Determination Of Parameters ◽  
Development And Validation

Abstract Background Standardization of polyherbal medicine though being the need of the hour is a toilsome task. Among the various methods employed for quality control and standardization of polyherbal medicine, phytochemical profiling is of utmost importance as it signifies the quality as well as efficacy of the medicine. The work was aimed to develop and validate a simple, quick, and accurate RP-HPLC technique for simultaneous assessment of monoammonium glycyrrhizinate and sennoside-B in a polyherbal laxative tablet. The phytomarkers were effectively quantified by RP-HPLC system on C18 analytical column using gradient mobile phase consisting of phosphate buffer to acetonitrile with the detector wavelength set at 254 nm. This developed method was validated by determination of parameters like accuracy, linearity, precision, limit of detection, and quantification as well as robustness according to ICH guidelines. Results Calibration curve of both phytomarkers showed excellent linear correlation coefficients. LOD and LOQ were also calculated by equation. Precision studies were carried out using intra-day and inter-day intervals and RSD values were found to be less than 2.00%. The method was found to be accurate, which was evident from 98.96 to 101.39% and 99.17 to 100.67% recovery of monoammonium glycyrrhizinate and sennoside-B, respectively, when the formulation was spiked with the respective phytomarkers. Conclusion The validated method can be employed as standardization tool for herbal formulations with accuracy and precision. The developed method will assist in maintaining the good quality and batch to batch uniformity of polyherbal formulations containing Yashtimadhu, Swarnpatri, and Aragvadha as active ingredients.

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