Patulin in apple and apple juice: Method development, validation by liquid chromatography-tandem mass spectrometry and survey in Brazilian south supermarkets

2019 ◽  
Vol 82 ◽  
pp. 103242 ◽  
Author(s):  
Jonatan V. Dias ◽  
Rosselei C. da Silva ◽  
Ionara R. Pizzutti ◽  
Ingrid D. dos Santos ◽  
Micheli Dassi ◽  
...  
2020 ◽  
Vol 58 (6) ◽  
pp. 1002-1009 ◽  
Author(s):  
Caroline Le Goff ◽  
Jordi Farre-Segura ◽  
Violeta Stojkovic ◽  
Patrice Dufour ◽  
Stéphanie Peeters ◽  
...  

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.


Author(s):  
L J Owen ◽  
B G Keevil

Background Testosterone measurement by liquid chromatography tandem mass spectrometry (LC-MS/MS) is well accepted as the preferred technique for the analysis of testosterone. Variation is seen between assays and is likely to be due to method differences. One area of inconsistency among assays is the choice of internal standard. We investigated the effects of three internal standards. Methods Testosterone with two deuterium (D2), five deuterium (D5) and three carbon 13 enrichment (C13) were separately assessed. Samples were extracted using ether following the addition of 10 μL of internal standard. All aliquots were prepared in triplicate, one for each type of internal standard. After mixing, the ether was transferred to a 96-deep well block, and then evaporated to dryness. Extracts were reconstituted with 50% mobile phases and analysed using a Waters Acquity UPLC and Quattro Premier tandem mass spectrometer. This method had previously been shown to have excellent agreement with a reference method using the D2 internal standard and this was considered the target. Results Lower results were obtained when using D5 testosterone when compared with D2 testosterone. The C13 internal standard also gave lower results, but was closer to the D2 target than the D5 internal standard. Conclusions The choice of internal standard alone can have a significant affect on the results obtained by LC-MS/MS assays for testosterone using this chromatography. The effects of the combination of chromatography and internal standard choice should be investigated during method development.


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