scholarly journals Development of a highly sensitive gas chromatography–mass spectrometry method preceded by solid‐phase microextraction for the analysis of propofol in low‐volume cerebral microdialysate samples

2019 ◽  
Vol 42 (6) ◽  
pp. 1257-1264 ◽  
Author(s):  
Armin Sebastian Guntner ◽  
Simon Stöcklegger ◽  
Michael Kneidinger ◽  
Udo Illievich ◽  
Wolfgang Buchberger
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Spectrometry Method ◽  
Mass Spectrometry Method ◽  
Chromatography Mass Spectrometry ◽  
Highly Sensitive ◽  
Low Volume

scholarly journals Sensitive Gas Chromatography-Mass Spectrometry Method for Simultaneous Measurement of MDEA, MDMA, and Metabolites HMA, MDA, and HMMA in Human Urine

2006 ◽  
Vol 52 (9) ◽  
pp. 1728-1734 ◽  
Author(s):  
Stephane O Pirnay ◽  
Tsadik T Abraham ◽  
Marilyn A Huestis
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Human Urine ◽  
Simultaneous Measurement ◽  
Dynamic Range ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Spectrometry Method ◽  
Mass Spectrometry Method ◽  
Chromatography Mass Spectrometry

Abstract Background: A sensitive gas chromatography-mass spectrometry method was developed and validated for the simultaneous measurement of MDEA, MDMA, and its metabolites, 3,4-methylenedioxy-N-ethylamphetamine (MDEA), 3,4-methylenedioxymethamphetamine (MDMA or Ecstasy), and its metabolites, 4-hydroxy-3-methoxyamphetamine (HMA), 3,4-methylenedioxyamphetamine (MDA), and 4-hydroxy-3-methoxyamphetamine (HMMA) in human urine. Methods: We hydrolyzed 1 mL urine, fortified with MDMA-d5, MDA-d5, and MDEA-d6, with 100 μL of concentrated hydrochloric acid at 120 °C for 40 min, then added 100 μL 10 N sodium hydroxide and 3 mL phosphate buffer 0.1 N (pH 6.0) were added to hydrolyzed urine specimens before solid-phase extraction. After elution and evaporation, we derivatized extracts with heptafluorobutyric acid anhydride and analyzed with gas chromatography-mass spectrometry operated in EI-selected ion-monitoring mode. Results: Limits of quantification were 25 μg/L for MDEA, MDMA, and its metabolites. Calibration curves were linear to 5000 μg/L for MDEA, MDMA, HMA, MDA, and HMMA, with a minimum r2 > 0.99. At 3 concentrations spanning the linear dynamic range of the assay, mean overall extraction efficiencies from urine were >85.5% for all compounds of interest. Intra- and interassay imprecisions, produced as CV, were <15% for all drugs at 30, 300, and 3000 μg/L. Conclusions: This gas chromatography-mass spectrometry assay provides adequate sensitivity and performance characteristics for the simultaneous quantification of MDEA, MDMA, and its metabolites HMMA, MDA, and HMA in human urine. The method meets and exceeds the requirements of the proposed Substance Abuse and Mental Health Services Administration’s guidelines for federal workplace drug testing of MDEA and MDMA in urine.

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