Ultra Fast Liquid Chromatography-Tandem Mass Spectrometry Routine Method for Simultaneous Determination of Cyclosporin A, Tacrolimus, Sirolimus, and Everolimus in Whole Blood Using Deuterated Internal Standards for Cyclosporin A and Everolimus

2010 ◽  
Vol 32 (1) ◽  
pp. 61-66 ◽  
Author(s):  
Andreas Meinitzer ◽  
Gabriele Gartner ◽  
Stefan Pilz ◽  
Mariana Stettin
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Cyclosporin A ◽  
Tandem Mass ◽  
Routine Method ◽  
Internal Standards ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Fast Liquid Chromatography

scholarly journals Measurement of Urinary d- and l-2-Hydroxyglutarate Enantiomers by Stable-Isotope-Dilution Liquid Chromatography–Tandem Mass Spectrometry after Derivatization with Diacetyl-l-Tartaric Anhydride

2004 ◽  
Vol 50 (8) ◽  
pp. 1391-1395 ◽  
Author(s):  
Eduard A Struys ◽  
Erwin E W Jansen ◽  
Nanda M Verhoeven ◽  
Cornelis Jakobs
Keyword(s):  
Mass Spectrometry ◽  
Differential Diagnosis ◽  
Liquid Chromatography ◽  
Stable Isotope ◽  
Tandem Mass Spectrometry ◽  
Tandem Mass ◽  
Internal Standards ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Abstract Background: The differential diagnosis of d-2-hydroxyglutaric aciduria (d-2-HGA), l-2-hydroxyglutaric aciduria (l-2-HGA), and the combined d/l-2-hydroxyglutaric aciduria (d/l-2-HGA) can be accomplished only by the measurement of the corresponding 2-hydroxyglutarate (2-HG). Available methods for the determination of d- and l-2-HG in urine are either time-consuming and expensive or have not been extensively validated. We aimed to develop a method for their rapid and sensitive measurement. Methods: We used liquid chromatography–tandem mass spectrometry (LC-MS/MS) for the determination of d- and l-2-HG with stable-isotope-labeled internal standards. Urine samples of 20 μL were mixed with 250 μL of methanol containing the internal standards and subsequently dried under nitrogen. The analytes were derivatized by use of diacetyl-l-tartaric anhydride (DATAN) to obtain diastereomers, which were separated on an achiral C18 HPLC column and detected by MS/MS in multiple-reaction-monitoring mode. Results: The use of DATAN as chiral derivatization reagent provided very well separated peaks of the formed diastereomers of d- and l-2-HG, with a total runtime of 5 min. The inter- and intraassay CVs for d- and l-2-HG ranged from 3.4% to 6.2%. Mean recoveries of d- and l-2-HG, evaluated on two concentrations, were 94%. Detection limit of the presented method was 20 pmol for a sample volume of 20 μL. Method comparison of the LC-MS/MS method with a gas chromatography–mass spectrometry method, in which d- and l-2-HG were derivatized with R-(−)-butanol, showed good agreement between the two methods. Conclusions: Urinary d- and l-2-HG can be analyzed by MS/MS after derivatization with DATAN. The presented method may be suitable for the differential diagnosis of 2-HGA.

Evaluation of the MassTrak Immunosuppressant XE Kit for the determination of everolimus and cyclosporin A in human whole blood employing isotopically labeled internal standards

2011 ◽  
Vol 49 (12) ◽  
Author(s):  
Misuk Ji ◽  
Sollip Kim ◽  
Hee-Jung Chung ◽  
Woochang Lee ◽  
Sail Chun ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Cyclosporin A ◽  
Therapeutic Drug ◽  
Tandem Mass ◽  
Transplant Recipients ◽  
Internal Standards ◽  
Human Whole Blood ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

AbstractLiquid chromatography-tandem mass spectrometry (LC-MS/MS) is widely used for therapeutic drug monitoring of immunosuppressants given to transplant recipients. This study evaluated the performance of the newly introduced MassTrak Immunosuppressant XE Kit (Waters Corporation; “the Kit”) in the determination of everolimus and cyclosporin A (CsA) using LC-MS/MS.The linearity, precision, detection limit, carryover and matrix effect of the Kit and comparison of the in-house method and Kit procedure were evaluated according to Clinical and Laboratory Standards Institute guidelines.The Kit afforded good linearity in the measurement of everolimus from 2 to 26 ng/mL (RThe Kit employing isotopically labeled internal standards provides reliable measurements of immunosuppressant levels over a broad range of concentrations.

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