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.

scholarly journals Ultrasound Assisted Method Development for the Determination of Selected Sulfonamides in Honey Using Liquid Chromatography-Tandem Mass Spectrometry

2016 ◽  
Vol 16 (2) ◽  
pp. 289-295
Author(s):  
M. Manimekalai ◽  
Anand Sheshadri ◽  
K. Suresh Kumar ◽  
Ashish Rawson
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Method Development ◽  
Age Groups ◽  
Veterinary Drug ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Honey is a highly valuable natural product, which is consumed by people of all age groups unaware of the high load of veterinary drug residues present. Sulfonamides are one such class of veterinary drugs, which are used in apiculture in higher amounts and impose a lot of negative health effects. This paper describes an analytical method developed for simultaneous determination of two Sulfonamides (Sulfamethizole and Trimethoprim) in honey using liquid chromatography- tandem mass spectrometry (LC-MS/MS). Suitable fragmentor voltage and collision energy were optimised for both the analytes. Five different sample preparation techniques based on ultrasonication were evaluated. In which ultrasonication at 80% amplitude, 5 minutes at 45°C gave improved recoveries. On validation, the developed method showed good linearity with r2 values in the range of 0.98-0.99 for both the sulfonamides. The effect of matrix on the method developed was evaluated and was found that the sample matrix does not pose considerable interferences with excellent linearities with r2 values above 0.95 for both the analytes. The method developed was found to be very selective and can find application in routine analysis for the determination of sulfonamides from honey samples.

scholarly journals METHOD DEVELOPMENT AND VALIDATION STUDY FOR QUANTITATIVE DETERMINATION OF GENOTOXIC IMPURITY AND ITS PRECURSOR IN FLUCONAZOLE SAMPLE BY LIQUID CHROMATOGRAPHY–TANDEM MASS SPECTROMETRY

2016 ◽  
Vol 8 (12) ◽  
pp. 84
Author(s):  
L. Narasimha Rao K ◽  
N. Devanna ◽  
K.v.n. Suresh Reddy
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Method Development ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Method Development And Validation ◽  
Development And Validation

<p><strong>Objective: </strong>The objective of this work is method development and validation study for quantitative determination of 1-[2-(2,4-difluorophenyl)-2,3-epoxypropyl]-1H-1,2,4-triazole, a genotoxic impurity and its precursor in a fluconazole drug sample by liquid chromatography–tandem mass spectrometry.</p><p><strong>Methods: </strong>LC-MS/MS analysis of these impurities was performed on Hypersil BDS C18 (100 mm x 4.0 mm, 3 µm) column. 5 mmol ammonium acetate and acetonitrile in the ratio of 65:35 (v/v) was used as the mobile phase with a flow rate of 0.4 ml/min. The developed method was accomplished with a short run time of 10 min. Triple quadrupole mass detector coupled with positive electrospray ionization was used for the quantification of genotoxic impurities in multiple reaction monitoring (MRM).</p><p><strong>Results: </strong>The method was validated as per International Conference on Harmonization (ICH) guidelines. The method was linear in the range of 0.30 µg/g to 11.37 µg/g for impurity A and 0.30 µg/g to 11.34 µg/g for impurity B with a correlation coefficient of 0.999. The accuracy of the method was in the range of 98.25 % to 100.53 % for both impurities.</p><p><strong>Conclusion: </strong>A specific, selective, highly sensitive and more accurate analytical method using LC-MS/MS coupled with positive electrospray ionization has been developed for the quantification of genotoxic impurity (1-[2-(2,4-difluorophenyl)-2,3-epoxypropyl]-1H-1,2,4-triazole) and its precursor (1-(2,4-difluorophenyl)-2-[1,2,4]triazol-1-yl-ethanone) at 0.3 µg/g with respect to the 5.0 mg/ml of fluconazole.</p>

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