超高效液相色谱-质谱联用法测定饮料中γ-羟基丁酸及其前体物质γ-丁内酯和1,4-丁二醇

Determination of γ-hydroxybutyrate and its precursor substances γ-butyrolactone,1,4-butanediol in beverages via ultra high performance liquid chromatography-mass spectrometry

建立了γ－羟基丁酸（GHB）及其前体物质γ－丁内酯（GBL）和1，4－丁二醇（1，4-BD）超高效液相色谱－质谱联用（UPLC-MS／MS）定性定量的检测方法。样品经滤膜过滤，使用Waters Atlantis T3色谱柱（2．1×150mm．3．0μm），以甲醇一水为流动相梯度洗脱，流速为0．25mL／min，串联质谱MRM模式检测，在3min内完成有效分离。采用外标法定量，GHB在0．1～5．0mg／L范围内线性良好（r〉0．999），GBL和1，4-BD在0．5～10．0mg／L范围内线性良好（r〉0．996），3种物质的检出限为20～50μg/L，定量下限为50～200μg／L，日内RSD和日间RSD小于7．6％。考察了不同饮料的基质和pH对目标物保留时间和峰面积的影响，提出了消除基质效应影响的建议，使其适用于实际案件侦破中非法添加GHB及其前体物质的定性及定量检测。

A uhra-high performance liquid chromatography coupled with triple quadruple tandem mass spectrometric （UPLC-MS/MS） method for the qualitative and quantitative determination of γ-hydroxybutyrate （GHB）, γ-butyrolactone （GBL） and 1,4-butanediol （1,4-BD） in beverage was established. After filtered with 0.22 ixm membrane, three target compounds were separated in 3 minutes on a Waters Atlantis T 3 column （2. 1 × 150 mm, 3.0 μm; Waters, Milford, MA, USA） with gradient elution using water （A） and methanol （B） at 0.25 mL/min. Samples were monitored via the ESI^＋ ionization mode and quantified by multiple reaction monitoring （MRM） model. The calibration curve was performed and good linear relationship （R ≥0. 99 ） was obtained with the concentration ranges of 0. 1 -5.0 mg/mL for GHB and 0. 5 - 10.0 mg/mL for GBL and 1,4- BD. The limits of detection（LOD） rangeed from 20-50 μg/L and limits of quantity（LOQ） rangeed from 50 to 200 μg/L. The relative standard deviations （RSD） of intra-day and inter-day were less than 7.6% in UPLC/ MS/MS. This method is simple, rapid and has high sensitivity, which can be applied to determination of illegal addition of GHB and its precursor substances in beverages. At the same time, the influence of the matrix effects and different pH value of beverages on the retention time and peak area were investigated and eliminated.