Reversed-Phase High Performance Liquid Chromatographic Analysis of Three First Line Anti-Tuberculosis Drugs

2019 ◽  
Vol 69 (12) ◽  
pp. 3590-3592
Author(s):  
Nela Bibire ◽  
Romeo Iulian Olariu ◽  
Luminita Agoroaei ◽  
Madalina Vieriu ◽  
Alina Diana Panainte ◽  
...  
Keyword(s):  
High Performance ◽  
Biological Fluids ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Assay Method ◽  
Active Pharmaceutical Ingredients ◽  
First Line ◽  
Pharmaceutical Ingredients ◽  
Liquid Chromatographic

Active pharmaceutical ingredients such as isoniazid, pyrazinamide and rifampicin are among the most important first-line anti-tuberculosis drugs. A simple, rapid and sensitive reversed phase-high performance liquid chromatographic assay method for the simultaneous determination of isoniazid, pyrazinamide and rifampicin has been developed. Separation of the interest compounds was achieved in a 10 min chromatographic run in gradient elution mode on a Zorbax SB-C18 stainless steel column (150 � 4 mm, 5 mm) using a guard column containing the same stationary phase. The gradient elution was carried out with a mobile phase of 10% CH3CN aqueous solution for channel A and 50% CH3CN in pH = 6.8 phosphate buffer (20 mM), to which 1.5 mL triethylamine were added for channel B. Quantification of the analyzed substances was carried out spectrophotometrically at 269 nm. Detection limits of 0.48 mg/L for isoniazid, 0.52 mg/L for pyrazinamide and 0.48 mg/L for rifampicin were established for the developed assay method. The present work showed that the proposed analysis method was advantageous for simple and rapid analysis of the active pharmaceutical ingredients in pharmaceuticals and biological fluids.

scholarly journals Constituents of Da-Cheng-Qi Decoction and its Parent Herbal Medicines Determined by LC-MS/MS

2010 ◽  
Vol 5 (5) ◽  
pp. 1934578X1000500
Author(s):  
Fengguo Xu ◽  
Ying Liu ◽  
Rui Song ◽  
Haijuan Dong ◽  
Zunjian Zhang
Keyword(s):  
High Performance ◽  
Herbal Medicines ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Esi Ms ◽  
Chemical Constitution ◽  
Tandem Mass Spectrometric ◽  
Liquid Chromatographic ◽  
First Time

Da-Cheng-Qi decoction (DCQD) is a purgative prescription used in China and East Asia. To profile the constituents of this complex traditional Chinese medicine (TCM), a high-performance liquid chromatographic, electrospray ionization, tandem mass spectrometric (HPLC-ESI/MS/MS) analytical method was developed. After separation on a reversed-phase C18 analytical column using gradient elution, samples were analyzed by ESI-MS/MS in negative mode. As a result, a total of 37 compounds were detected, of which two tannins, three anthraquinones, two sennosides, five flavonoids and two lignans were unambiguously identified by comparison with standard compounds, and sixteen compounds were either tentatively identified or deduced according to their MS/MS data. The fragmentation pathways of many of the observed compounds, such as the tannins and lignans are reported for the first time. In addition, the identity of each peak in DCQD was explored by comparison with those of its three constituent herbs. The results indicated that tannins, anthraquinones and sennosides in DCQD originated from Radix et Rhizoma Rhei, flavonoids from Fructus Aurantii Immaturus, and lignans from Cortex Magnoliae officinalis. The present study provides an example of chemical constitution profiling in complex TCM systems using LC/MS/MS.

scholarly journals A Stability-Indicating High-Performance Liquid Chromatographic Method for the Determination of Methocarbamol in Veterinary Preparations

2009 ◽  
Vol 92 (5) ◽  
pp. 1602-1606 ◽  
Author(s):  
María A Rosasco ◽  
Rita Ceresole ◽  
Clara C Forastieri ◽  
Adriana I Segall
Keyword(s):  
High Performance ◽  
Uv Light ◽  
Degradation Products ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Assay Method ◽  
Liquid Chromatographic Method ◽  
Validation Parameters ◽  
Liquid Chromatographic

Abstract An isocratic HPLC method was developed and validated for the quantitation of methocarbamol in the presence of its degradation products. Quantitation was achieved using a reversed-phase C18 column at ambient temperature with mobile phase consisting of methanolwatertetrahydrofuran (25 + 65 + 10, v/v). The flow rate was 0.9 mL/min. The detection was by UV light at 274 nm. The proposed method was validated for selectivity, precision, linearity, and accuracy. The assay method was found to be linear from 159.0 to 793.2 g/mL (3.2 to 15.9 g injected). All validation parameters were within the acceptable range. The developed method was successfully applied to estimate the amount of methocarbamol in a veterinary injection.

Liquid-chromatographic assay of cefamandole in serum, urine, and dialysis fluid.

1986 ◽  
Vol 32 (1) ◽  
pp. 197-200 ◽  
Author(s):  
M Bliss ◽  
M Mayersohn
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Biological Fluids ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Pharmacokinetic Studies ◽  
Dialysis Fluid ◽  
Serum Samples ◽  
Liquid Chromatographic ◽  
Phase Column

Abstract We describe a "high-performance" liquid-chromatographic assay for quantifying cefamandole in biological fluids from patients with renal impairment. Serum samples are deproteinized with acetonitrile, then extracted with dichloromethane; dialysis-fluid samples are injected directly; urine samples are diluted appropriately before injection onto the reversed-phase column. The mobile phase is a methanol/aqueous solution (31/69 by vol) containing 500 microL of phosphoric acid, 20 mmol of sodium sulfate, and 200 microL of triethylamine per liter, the mixture being adjusted to pH 6.0 with NaOH. Retention time for cefamandole is 12 min. Its peak is well resolved in highly contaminated samples from renally impaired subjects. The assay's selectivity, reproducibility (within-day and between-day CVs less than 8% in all three sample fluids), and sensitivity--0.5 mg/L in serum, 1.0 mg/L in dialysis fluid, and 5.0 mg/L in urine--make it applicable to pharmacokinetic studies.

scholarly journals DETERMINATION OF 5H-BENZO[2,3][1,4]OXAZEPINO[5,6-B]INDOLES IN RAT PLASMA BY REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC-ULTRAVIOLET METHOD: APPLICATION TO PHARMACOKINETIC STUDIES

2017 ◽  
Vol 10 (12) ◽  
pp. 425 ◽  
Author(s):  
Ashok K Singh ◽  
Vinit Raj ◽  
Amit Rai ◽  
Amit K Keshari ◽  
Pranesh Kumar ◽  
...  
Keyword(s):  
High Performance ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Rat Plasma ◽  
Reversed Phase ◽  
Pharmacokinetic Studies ◽  
Relative Standard ◽  
Liquid Chromatographic

Objective: Recently, we reported newly synthesized 5H-benzo[2,3][1,4]oxazepino[5,6-b]indole) derivatives and proved their cytotoxicity against hepatocellular carcinoma specific Hep-G2 cell lines. We attempted herein to describe a reversed-phase high-performance liquid chromatographic method for the determination of three most active compounds 6a, 10a, and 15a in rat plasma to predict their pharmacokinetics parameters before in vivo study.Methods: A rapid and sensitive reversed-phase high-performance liquid chromatographic was employed for the determination of 6a, 10a, and 15a in rat plasma. Each compound was separated by a gradient elution of acetonitrile and water with 1 mL/min flow rate. The detector was set at 270, 285, and 275 nm for 6a, 10a, and 15a and the recorded elution times were 2.00, 2.87, and 1.88 min, respectively.Results: The calibration curve was linear with R2 of 0.938, 0.875, and 0.923 over the concentration range of 0.1–50 μg/mL. The inter- and intra-day variations of the assay were lower than 12.26%; the average recovery of 6a, 10a, and 15a was 97.31, 92.56, and 95.23 % with relative standard deviation of 2.12%, 3.25%, and 2.28%, respectively. The Cmax and Tmax were ~ 46.34, 18.56, and 25.65 μg/mL and 2.0, 4.0, and 4.0 h for 6a, 10a, and 15a, respectively, which indicate a robust method of detection in the present experiment.Conclusion: The study suggests that all of the three compounds have a lower rate of absorption, higher volume of distribution, and lower clearance rate, indicating good therapeutic response for in vivo activity. 

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