scholarly journals Detection and development of a quantitation method for undeclared compounds in antidiabetic biologically active additives and its validation by high performance liquid chromatography

Pharmacia ◽  
2022 ◽  
Vol 69 (1) ◽  
pp. 45-50
Author(s):  
Virab Gurgen Kirakosyan ◽  
Avetis Hovhannes Tsaturyan ◽  
Lilit Eduard Poghosyan ◽  
Ella Vardan Minasyan ◽  
Hayk Razmik Petrosyan ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Sodium Dodecyl ◽  
Biologically Active ◽  
Ich Guidelines ◽  
System Suitability ◽  
Precision And Accuracy ◽  
Quantitation Method

An isocratic, high-performance liquid chromatography (HPLC) quantitation method was developed for the quantitative determination of metformin, glibenclamide, gliclazide, glimepiride in some antidiabetic biologically active additives. A Nucleosil C18, 5 μm, 4.6 mm × 150 mm, column with mobile phase containing buffer (10 mm Na2HPO4, 10 mm sodium dodecyl sulfate): acetonitrile = 68 : 32 (V/V), pH = 7.5 was used. The flow rate was 1.0 mL/min, and effluents were monitored at 226 nm. The retention times of gliclazide glibenclamide, glimepiride and metformin, were 2.203, 4.587, 5.667 and 10.182 min, respectively. Linearity was studied by preparing standard solutions of gliclazide, glibenclamide, glimepiride and metformin at the concentration range of 50% to 150% of working concentration from a stock solution. The method was successfully applied to the estimation of gliclazide, glibenclamide, glimepiride and metformin in some antidiabetic biologically active additives. This method was validated to confirm its system suitability, selectivity, linearity, precision and accuracy according to international conference on harmonization (ICH) guidelines.

scholarly journals A microemulsion high-performance liquid chromatography (MELC) method for the separation and determination of hydrolyzed tenuifolin in Radix Polygalae

2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Hui Yan ◽  
Zhuan-Di Zheng ◽  
Hong-Fei Wu ◽  
Xiao-Chuang Liu ◽  
An Zhou
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Limit Of Quantification ◽  
Analyte Molecule ◽  
Oil In Water

AbstractTenuifolin was used as a reliable chemical marker for the quality control of Radix Polygalae. The determination of tenuifolin is challenging because the analyte molecule lacks a suitable chromophore. The aim of this study was to establish a microemulsion high-performance liquid chromatography (MELC) method which is robust and sensitive, and can separate and determine tenuifolin in Radix Polygalae using an oil-in-water (O/W) microemulsion mobile phase. The separations were performed on a C18 (4.6 × 250 mm, 5 μm) column at 25 °C using a flow rate of 1.0 mL/min, and an ultraviolet detection wavelength of 210 nm. The microemulsion mobile phase comprised 2.8% (w/v) sodium dodecyl sulfate (SDS), 7.0% (v/v) n-butanol, 0.8% (v/v) n-octane and 0.1% (v/v) aqueous orthophosphate buffer (H3PO4). The linearity analysis of tenuifolin showed a correlation coefficient of 0.9923 in the concentration range of 48.00–960.00 µg/mL. The accuracy of the method based on three concentration levels ranged from 96.23% to 99.28%; the limit of detection (LOD) was 2.34 µg/mL, and the limit of quantification (LOQ) was 6.76 µg/mL. The results of our study indicated that the optimized MELC method was sensitive and robust, and can be widely applied for the separation and determination of tenuifolin in Radix Polygalae.

scholarly journals Determination of Benzalkonium Chloride in Nasal Drops by High-Performance Liquid Chromatography

2012 ◽  
Vol 9 (3) ◽  
pp. 1599-1604 ◽  
Author(s):  
Danijela A. Kostić ◽  
Snezana S. Mitić ◽  
Danijela Č. Nasković ◽  
Aleksandra R. Zarubica ◽  
Milan N. Mitic
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Benzalkonium Chloride ◽  
High Performance ◽  
Reversed Phase ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Acceptance Range

A high-performance liquid chromatography (HPLC) system was used in the reversed phase mode for the determination of benzalkonium chloride (BKC) in nosal drops. A Chromolit RP-18e, 100 x 4.6, (UM6077/035) column was used at 40 °C. The mobile phase, optimized through an experimental design, was a 70:30 (v/v) mixture of 0.057M Na-heksansulphonate potassium, dihydrogen orthophosphate buffer (pH 2.9) and acetonitrile, pumped at a flow rate of 1.75 mL/min at maintaining column temperature at 40 °C. Maximum UV detection was achieved at 215 nm. The method was validated in terms of selectivity, linearity, repeatability, precision and accuracy. The method was successfully applied for the determination of BKC in a pharmaceutical formulation of nasal drop solution without any interference from common excipients and drug substance. All the validation parameters were within the acceptance range, concordant to ICH guidelines.

scholarly journals Development of a rapid and reliable high-performance liquid chromatography method for determination of water-soluble vitamins in veterinary feed premix

2021 ◽  
pp. 3084-3090
Author(s):  
Md. Zahangir Hosain ◽  
S. M. Shariful Islam ◽  
Md. Mostofa Kamal
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Water Soluble ◽  
Dihydrogen Phosphate ◽  
Chromatography Method ◽  
System Suitability ◽  
Relative Standard ◽  
Feed Premix

Background and Aim: Determination of trace amounts of vitamins in multi-component feed premix is a troublesome analytical procedure. In this study, a simple and rapid high-performance liquid chromatography (HPLC) method was developed and validated for the concurrent detection and quantitation of four water-soluble vitamins such as thiamine, riboflavin, pyridoxine, and cyanocobalamin in veterinary feed premixes. Materials and Methods: The chromatographic separation of the vitamins was carried out at 35°C temperature on a reversed-phase C18 column using a gradient pump mode. Mobile phase constituents were solvent (a): 25 mM Potassium dihydrogen phosphate and 5 mM sodium hexanesulfonate in deionized water having pH-4.0 and solvent and (b) 5 mM sodium hexanesulfonate in methanol. Detection was performed with HPLC ultraviolet/visible detection set at 278 and 361 nm wavelength in two different channels. The flow rate was 1.2 mL/min and the total run time was 25 min. Results: The method was validated according to the International Conference on Harmonization and Food and Drug Administration guidelines and acceptance criteria for system suitability, precision, linearity, and recovery were met in all cases. The relative standard deviation for system suitability and precision was <2% for all vitamins. The linearity of the calibration curves was excellent (R2>0.999) at concentration of 5, 10, 15, 20, 25, and 30 μg/mL for all vitamins. The limits of detection values were 0.0125, 0.0017, 0.0064, and 0.0065 μg/mL for thiamine, riboflavin, pyridoxine, and cyanocobalamin, respectively, and the limits of quantification values were 0.0378, 0.0051, 0.0213, and 0.0198 μg/mL for thiamine, riboflavin, pyridoxine, and cyanocobalamin, respectively. The recovery percentages ranged from 88% to 115%. Conclusion: The overall parameters of the proposed method met the validation criteria and this method could be a highly desirable technique for routine analysis of water-soluble vitamins in veterinary feed premix.

scholarly journals Development and validation of a single HPLC method for the determination of thirteen pharmaceuticals in bulk and tablet dosage form

2021 ◽  
Vol 35 (1) ◽  
pp. 17-31
Author(s):  
B. Tegegne ◽  
B. S. Chandravanshi ◽  
F. Zewge ◽  
L. Pillay ◽  
L. Chimuka
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Hplc Method ◽  
Mobile Phase Flow Rate ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Tablet Dosage

The aim of this study was to develop and validate a high performance liquid chromatography (HPLC) method for the determination of thirteen selected pharmaceutical compounds (metformin, amoxicillin, chloroquine, theophylline, trimethoprim, caffeine, norfloxacin, ciprofloxacin, acetylsalicylic acid, doxycycline hyclate, metronidazole, albendazole and cloxacillin) in bulk and tablet dosage form. Chromatographic separation using a Kromasil C18 column, gradient elution with aqueous formic acid (0.1%), methanol and acetonitrile, a UV absorption wavelength of 250 nm and a mobile phase flow rate of 1 mL/min over a 22 min run time was optimized for complete separation of the selected target compounds. The method was validated and results for: linearity, precision, sensitivity, accuracy, specificity, suitability and method robustness were obtained and met the ICH guidelines. Calibration curve correlation coefficients ranged from 0.9985-0.9998 and the percentage relative standard deviations for repeated analysis was below 5%, indicating acceptable method precision. The limits of detection (LODs) and quantification (LOQs) ranged from 0.020-0.27 µg/L and 0.080-0.91 µg/L, respectively. The accuracy study yielded recoveries in the ranges 86.0-102% for pure compounds and 90.9-106% for compounds in tablet dosage form. The method is robust for small or deliberate changes to the chromatographic parameters and found to be appropriate for analysis of tablets for the determination of the thirteen pharmaceuticals.                     KEY WORDS: Pharmaceuticals, Bulk determination, Tablet dosage, High performance liquid chromatography, Method development, ICH guidelines   Bull. Chem. Soc. Ethiop. 2021, 35(1), 17-31. DOI: https://dx.doi.org/10.4314/bcse.v35i1.2

scholarly journals A novel simultaneous high performance liquid chromatography-PDA method for the determination of Tenofovir AF, Darunavir, Emtricitabine and Cobicistat in bulk and its application to marketed formulation

2022 ◽  
Vol 8 (1) ◽  
Author(s):  
Challamalla Pavani ◽  
E. Susithra
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Volume Ratio ◽  
Quantitation Limit ◽  
Ich Guidelines ◽  
Tenofovir Alafenamide ◽  
Tablet Dosage

Abstract Background The present research article involves the simultaneous determination of Tenofovir alafenamide, Darunavir, Emtricitabine and Cobicistat in bulk as well as in tablet dosage form using high performance liquid chromatography. Result The separation was performed using DIKMA Spursil, C18, ODS, (4.6 × 150 mm × 5 µm) analytical column using the mobile phase acetonitrile and 0.1% Orthophosphoric acid in the volume ratio of 70:30 at pH 3. The eluents were detected using PDA detector at 254.0 nm. After optimization subsequent validation study of different parameters was performed by utilizing the optimised condition as per the ICH guidelines. Under this optimised conditions Tenofovir alafenamide, Darunavir, Emtricitabine and Cobicistat were eluted at 2.287 min, 2.507 min, 4.062 min, 6.011 min respectively. Percentage assay was found 99.21% for Tenofovir alafenamide, 99.80% for Darunavir, 99.80% for Emtricitabine and 99.84% for Cobicistat. Tenofovir alafenamide was found linear in the range of 2.0–10.0 µg/mL, Darunavir (160.0–800.0 µg/mL), Emtricitabine (40.0–200.0 µg/mL) and for cobicistat (30.0–150.0 µg/mL). The corelation coefficient was found 0.999 for all the APIs. The detection limit was found 0.14 µg/mL for Tenofovir alafenamide, 2.14 µg/mL for Darunavir, 0.6 µg/mL for Emtricitabine and 7.32 µg/mL for cobicistat. In the LOQ study the quantitation limit was found 0.47 µg/mL for Tenofovir alafenamide, 7.12 µg/mL for Darunavir, 2.10 µg/mL, for Emtricitabine and 24.42 µg/mL for cobicistat. Conclusion All the studied API’s has been highly resolute utilizing the optimised condition and found extremely suitable for the determination of all of them simultaneously in marketed dosage form as well as in the bulk form.

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