scholarly journals METHOD DEVELOPMENT AND VALIDATION OF LERCANIDIPINE IN HUMAN PLASMA BY LIQUID CHROMATOGRAPHY TANDEM-MASS SPECTROMETRY

2018 ◽  
Vol 10 (4) ◽  
pp. 87
Author(s):  
Yahdiana Harahap ◽  
Norma Andriyani ◽  
Harmita .
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Method Development ◽  
Matrix Effects ◽  
Multiple Reaction Monitoring ◽  
Tandem Mass ◽  
Mass Detection ◽  
Column Temperature ◽  
Z Value

Objective: To obtain an optimum and validated method for analyzing lercanidipine in plasma using Ultra Performance Liquid Chromatography of Tandem Mass Spectrometry (UPLC-MS/MS).Methods: The separation was carried out using 1.7μm (2.1 x 100 mm) Waters AcquityTM UPLC C18 column, a mobile phase of the 0.1% formic acid-methanol mixture (20:80 v/v) with isocratic elution, 30 °C column temperature, 0.2 ml/min flow rate and amlodipine as an internal standard. Mass detection was performed with a positive XBL TQD type Electrospray Ionization (ESI) in Multiple Reaction Monitoring modes. Lercanidipine was detected at m/z value of 612.11>280.27 and amlodipine was detected at m/z value 409.1>238.15. The optimum sample preparation method was a liquid-liquid extraction using 5 ml of n-hexane-ethyl acetate (50:50 v/v), vortex mixed for 3 min, centrifuged at 4000 rpm for 20 min, evaporated with nitrogen at 50 °C for 30 min, and the residue was reconstituted with 100 μl of mobile phase.Results: The method was linear in the range of 0.025-10 ng/ml with r ≥ 0.9986. Accuracy and precision within-run and between-run met the requirements with %diff and %CV, not exceeding ± 15% and not more than ± 20% for Lower Limit of Quantification (LLOQ) concentration.Conclusion: It was concluded that the developed method met the requirements of selectivity, carry over, stability, the integrity of dilution, and matrix effects under the Guideline on Bioanalytical Method Validation by the European Medicines Agency in 2011. 

scholarly journals BIOANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF CANAGLIFLOZIN IN HUMAN PLASMA BY LIQUID CHROMATOGRAPHY–TANDEM MASS SPECTROMETRY

2019 ◽  
pp. 46-51 ◽  
Author(s):  
DEEPAN T ◽  
BASAVESWARA RAO MV ◽  
DHANARAJU MD
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Plasma ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Objective: A validated liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed for canagliflozin in human plasma along with stability studies. Methods: The chromatographic separation of canagliflozin was performed on Zorbax XDB phenyl (75 × 4.6 mm, 3.5 mm) using methanol:acetate buffer (80:20 v/v) at a flow rate of 1.0 ml/min. The LC–MS/MS system consists of API 4000 triple quadrupole mass spectrometer equipped with turbospray ionization and an AS8020 automatic sample injector. Results: The retention time of canagliflozin was 1.15 min and total runtime was 2 min. The multiple reaction monitoring was 462.5/267.1 (m/z) for canagliflozin and 466.4/267.2 (m/z) for internal standard (canagliflozin D4), respectively. The method was linear over the range of 10–7505 ng/ml. The calculated slope ranged from 0.0451 to 0.0502 and intercepts from 0.0102 to 0.0456 with coefficients of the determination of 0.9970. The overall mean recovery of internal standard and canagliflozin was 76.66 and 79.77, respectively. Conclusion: The method was successfully validated and it was found to be within the limits for accuracy, precision, and linearity and it is stable under analytical conditions used.

scholarly journals Method Development and Validation of Darifenacin in Rat Plasma by Liquid Chromatography-Tandem Mass Spectrometry: Application to a Pharmacokinetic Study

2012 ◽  
Vol 2012 ◽  
pp. 1-9
Author(s):  
Thejomoorthy Karavadi ◽  
B. R. Challa
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Pharmacokinetic Study ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Rat Plasma ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

A selective, sensitive, and high-throughput liquid chromatography-tandem mass spectrometry (LC-ESI-MS/MS) method has been developed and validated for the quantitation of darifenacin in rat plasma. Sample clean up involved liquid-liquid extraction (LLE) and used 100 μL of rat plasma. Zorbax, SB C18, 4.6×75 mm, 3.5 μm particle size analytical column using 10 mM ammonium acetate buffer (pH 5) and methanol (10 : 90, v/v) as the mobile phase was used. The parent → product ion transitions for the drug (m/z 427.3 → 147.3) and IS (m/z 431.4 → 151.2) were monitored on a triple quadrupole mass spectrometer, operating in the multiple reaction monitoring (MRM) and positive ion mode. The method was validated over the concentration range of 10.00–20000.00 pg/mL for darifenacin. The method was successfully applied into a pharmacokinetic study in rat plasma under fasting conditions.

scholarly journals Determination of Pesticides in Soy-Based Infant Formula Using Liquid Chromatography with Electrospray Ionization Tandem Mass Spectrometry

2006 ◽  
Vol 89 (1) ◽  
pp. 214-224 ◽  
Author(s):  
Jian Wang ◽  
Wendy Cheung
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Electrospray Ionization ◽  
Infant Formula ◽  
Matrix Effects ◽  
Multiple Reaction Monitoring ◽  
Tandem Mass ◽  
Calibration Curves ◽  
Ionization Tandem Mass Spectrometry

Abstract A sensitive method using liquid chromatography with electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) was developed and validated to quantify and confirm 13 pesticides, including aldicarb sulfoxide, aldicarb sulfone, oxamyl, methomyl, formetanate, 3-hydroxycarbofuran, carbendazim, thiabendazole, aldicarb, propoxur, carbofuran, carbaryl, and methiocarb, in soy-based infant formula. Data acquisition under MS/MS was achieved by applying multiple reaction monitoring of 2 fragment ion transitions to provide a high degree of sensitivity and selectivity for both quantitation and confirmation. Different approaches to constructing calibration curves were compared and discussed to address issues of the extraction efficiency or recovery, and matrix effects. Matrix-matched standard calibration curves with the use of isoprocarb as an internal standard were finally used to achieve the best accuracy of the method. Under most circumstances, recoveries of 13 pesticides, spiked at 5.0, 25.0, and 45.0 g/kg, were close to 100%. The method detection limits (signal-to-noise ratio 3:1; g/kg) of 13 pesticides were 0.2 for thiabendazole and methiocarb, 0.6 for aldicarb, and 0.1 for the others.

scholarly journals The pathway through LC-MS method development: in-house or ready-to-use kit-based methods?

2020 ◽  
Vol 58 (6) ◽  
pp. 1002-1009 ◽  
Author(s):  
Caroline Le Goff ◽  
Jordi Farre-Segura ◽  
Violeta Stojkovic ◽  
Patrice Dufour ◽  
Stéphanie Peeters ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Method Development ◽  
Clinical Laboratory ◽  
Cross Reactivity ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

AbstractHistorically, the determination of low concentration analytes was initially made possible by the development of rapid and easy-to-perform immunoassays (IAs). Unfortunately, typical problems inherent to IA technologies rapidly appeared (e.g. elevated cost, cross-reactivity, lot-to-lot variability, etc.). In turn, liquid chromatography tandem mass spectrometry (LC-MS/MS) methods are sensitive and specific enough for such analyses. Therefore, they would seem to be the most promising candidates to replace IAs. There are two main choices when implementing a new LC-MS/MS method in a clinical laboratory: (1) Developing an in-house method or (2) purchasing ready-to-use kits. In this paper, we discuss some of the respective advantages, disadvantages and mandatory requirements of each choice. Additionally, we also share our experiences when developing an in-house method for cortisol determination and the implementation of an “ready-to-use” (RTU) kit for steroids analysis.

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