XU Manman, ZHAO Meng, WANG Zhaohong, LI Hong, DUAN Zhengping, WEN Yunbo
Abstract (
)
Download PDF
HTML
Knowledge map
Save
Objective To establish a method for the determination of γ-hydroxybutyric acid (GHB) and its precursors [1,4-butanediol (1,4-BD) and γ-butyrolactone (GBL)] in beverage or urine by ultra-high performance liquid chromatography coupling with the triple quadrupole tandem mass spectrometry, so as to provide technical support and appraisal basis for the detection of relevant cases. Methods With GHB-d6 as the internal standard, the sampling beverage or urine was diluted (1: 99) with 0.1% aqueous ammonia solution, afterwards centrifuged and filtered, consecutively having the resulted sample separated through an Acquity UPLC HSS T3 column (2.1mm×100mm, 1.8μm) that was eluted with ammonia water solution-methanol as the mobile phase. Each separated compound was detected with electrospray positive ionization (ESI+) and negative ionization (ESI-) in the MRM mode. Results The tested sample showed that the 3 compounds (GHB, 1,4-BD, GBL) were of good linear relationship in the range of 2-500μg/mL and the correlation coefficients of R2>0.997, with the spiked recoveries (R%) at three concentrations (low, medium, high ) being 86.6%-122.2%, the relative standard deviation (RSD%) being between 0.7% -9.2%. Besides, the detection limits of GHB and GBL were 1μg/mL, yet that of 1,4-BD was 2μg/mL. The quantitative limit of GHB was 2μg/ml, with that of GBL 2-3μg/mL and 1,4-BD’s 3-4μg/mL. Conclusions The method is of simple sample preparation, high recovery and high precision, capable of being used for the related cases to test γ-hydroxybutyric acid and its precursors in beverage or urine.