scholarly journals THE EFFECT OF ANTICOAGULANT TYPES ON THE IN VITRO ANALYSIS OF CLOPIDOGREL IN HUMAN PLASMA USING LIQUID CHROMATOGRAPHY TANDEM-MASS SPECTROMETRY

2018 ◽  
Vol 10 (1) ◽  
pp. 392
Author(s):  
Yahdiana Harahap ◽  
Anisa Maulidina ◽  
Delly Ramadon
Keyword(s):  
Liquid Chromatography ◽  
Internal Standard ◽  
Linear Calibration ◽  
Column Temperature ◽  
Heparin Plasma ◽  
Liquid Chromatography Tandem Mass ◽  
Edta Plasma ◽  
The Stability ◽  
Vitro Analysis

Objective: The aim of this study was to optimize and validate a plasma clopidogrel analysis method using liquid chromatography tandem-massspectrometry.Methods: Plasma samples were analyzed using a BEH C18 column (1.7 μm; 100 mm×2.1 mm), the mobile phase was 0.1% formic acid in acetonitrile(30:70, v/v). The flow rate was 0.2 mL/min, with a column temperature set to 35°C, an injection volume of 5 μL, an analysis time of 4 min, andirbesartan as the internal standard. Aliquots were obtained by liquid-liquid extraction using ammonium acetate and diethyl ether. The stability andpeak area ratio of the respective plasma area responses were evaluated using ANOVA.Results: No significant differences (p>0.05) were observed between anticoagulants regarding analyte stability. However, the peak area ratioshowed significant differences (p<0.05) between the anticoagulants. The accuracy and precision of the analysis with citrate, heparin, andethylenediaminetetraacetic acid (EDTA) plasma met the quality requirements, and a linear calibration curve was created with concentrations rangingfrom 0.02 to 5.0 ng/mL.Conclusion: The results showed that improved analysis of clopidogrel was achieved using citrate or heparin plasma compared with EDTA plasma.

scholarly journals Development of Liquid-Chromatography Tandem-Mass-Spectrometry Method for Determining Environmental Contamination by Powdered Medicinal Drugs in Pharmacies

2021 ◽  
Vol 58 ◽  
pp. 004695802110592
Author(s):  
Shiori Hasegawa ◽  
Ryoichi Inaba ◽  
Hiroki Nakamura ◽  
Yamato Kato ◽  
Satoshi Nakao ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Internal Standard ◽  
Tandem Mass ◽  
Linear Calibration ◽  
Ionization Source ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Medicinal Drugs

The environment and personnel are both exposed to powdered pharmaceuticals inside pharmacies. This makes developing new methods for rapidly determining such contaminants an important objective. In this study, we developed a liquid-chromatography tandem-mass-spectrometry (LC–MS/MS) method for the simultaneous qualitative and quantitative determination of powdered medicinal drugs, such as famotidine, risperidone, lansoprazole, olanzapine, haloperidol, clarithromycin, promethazine, levomepromazine, and chlorpromazine. The method involves the use of acetaminophen as the internal standard, an LC–MS/MS method with a core–shell column, and a 10 mM ammonium formate/acetonitrile gradient mobile phase. The analytes were separated within 14 min, and MS with an electrospray ionization source in positive-ion mode was used. The limits of detection for the 9 drugs were .1-8.4 ng/mL. Linear calibration curves in the 10-50 000 ng/mL range were constructed, and inter-day accuracies of 92.6-113.8% were determined for the 9 drugs. The coefficients of variation were less than 14.6%. These data suggest that the proposed method is applicable for the routine assaying of powdered-medicine contamination in pharmacies.

scholarly journals Development and validation of a liquid chromatography-tandem mass spectrometric method for the determination of lenalidomide in human plasma and its application on bioequivalence studies

2019 ◽  
Vol 10 (1) ◽  
Author(s):  
R. Gopinath ◽  
S. T. Narenderan ◽  
M. Kumar ◽  
B. Babu
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Internal Standard ◽  
Spectrometric Method ◽  
Tandem Mass ◽  
Mass Spectrometric Method ◽  
Mass Detection ◽  
Triple Quadrupole Mass Spectrometer ◽  
Liquid Chromatography Tandem Mass ◽  
Tandem Mass Spectrometric

AbstractA simple, sensitive, and specific liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) method was developed and validated for the quantification of lenalidomide in human plasma. The separation was carried out on a symmetry, C18, 5-μm (50 × 4.6 mm) column as stationary phase and with an isocratic mobile phase of 0.1% formic acid in water-methanol in the ratio of (15:85, v/v) at a flow rate of 0.5 mL/min. Protonated ions formed by electrospray ionization in the positive mode were used to detect analyte and fluconazole (internal standard). The mass detection was made by monitoring the fragmentation of m/z 260.1/148.8 for lenalidomide and m/z 307.1/238.0 for internal standard on a triple quadrupole mass spectrometer. The developed method was validated over the concentration range of 10–1000 ng/mL for lenalidomide in human plasma with a correlation coefficient (r2) was 0.9930. The accuracy and precision values obtained from six different sets of quality control samples analyzed on separate occasions ranged from 99.41 to 106.97% and 2.88 to 4.22%, respectively. Mean extraction recoveries were 98.06% and 88.78% for the analyte and IS, respectively. The developed method was successfully applied for analyzing lenalidomide in human plasma samples.

scholarly journals Development of a method for the measurement of dehydroepiandrosterone sulphate by liquid chromatography-tandem mass spectrometry

2005 ◽  
Vol 42 (6) ◽  
pp. 468-474 ◽  
Author(s):  
C A Chadwick ◽  
L J Owen ◽  
B G Keevil
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Lower Limit ◽  
Internal Standard ◽  
Tandem Mass ◽  
Dehydroepiandrosterone Sulphate ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Background: Dehydroepiandrosterone sulphate (DHEAS) is a steroid that is increasingly being recognized as a potential drug of abuse in many countries. This is due to its reputation as a hormone that may be able to retard the ageing process. The measurement of DHEAS is useful in the diagnosis of medical conditions such as congenital adrenal hyperplasia and polycystic ovary syndrome. Thus, a liquid chromatography-tandem mass spectrometry method has been developed to determine DHEAS concentrations in human serum. Method: The chromatography was performed using a WatersTM 2795 Alliance HT LC system coupled to a Mercury Fusion-RP column fitted with a SecurityGuardTM column. Results: DHEAS and the internal standard, deuterated DHEAS, both had a retention time of 1.5 min. The transition determined by the Micromass QuattroTM tandem mass spectrometer for DHEAS was m/z 367.3>96.7 and for the internal standard m/z 369.3>96.6. The method was linear up to 20 µmol/L; the lower limit of detection and the lower limit of quantitation were both 1 µmol/L. The intra- and interassay imprecision were <11% over a concentration range of 1-18 µmol/L for the in-house quality control and <12% for the intra- and interassay imprecision for the Bio-Rad Lyphocheck QC. Conclusion: The measurement of DHEAS by liquid chromatography-tandem mass spectrometry is robust and has a simple sample preparation procedure with a rapid cycle time of only 4 min.

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