建立了超高效液相色谱-串联质谱(ultimate performance liquid chromatography-mass spectrometry, UPLC-MS/MS)方法同时定性定量测定饮料中γ-羟基丁酸(γ-hydroxybutyrate, GHB)及其前体物质γ-丁内酯(γ-butyrolactone,GBL)和1,4-丁二醇(1,4-BD)。样品经适当倍数稀释,经0.22 μm滤膜过滤后,选用Thermo Gold C18色谱柱(150×2.1 mm,3.0 μm),以乙腈-2 mmol/L乙酸铵水溶液为流动相,梯度洗脱,流速为0.2 mL/min,采用Waters Xevo TQD超高效液相色谱-串联质谱仪的多反应监测(multiple reaction monitoring, MRM)扫描方式进行检测。试验表明,3种化合物在10 min内基线完全分离,峰型良好。采用外标法定量,GHB、GBL和1,4-BD在0.5～10.0 μg/mL范围内线性良好(r＞0.99),检出限为0.5 μg/mL。GHB的回收率为81.1%～87.7%,RSD为3.3%～5.7%(n=6),1,4-BD的回收率为98.5%～99.8%,RSD为3.7%～5.3%(n=6),GBL的回收率为107.5%～116.2%,RSD为3.5%～5.1%(n=6)。该方法精密度、重复性、稳定性及加标回收率的RSD均小于6%(n=6),所建立的方法灵敏度高、简便快速,能应用于不同饮料中目标物质的检测。
A ultimate performance liquid chromatography-mass spectrometry (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. The samples were diluted by different multiples and filtered with 0.22 μm membrane. Three compounds were separated in 10 minutes on a column of Thermo Gold C18(150×2.1 mm,3.0 μm) with gradient elution using 2 mmol/L ammonium acetate(A) and acetonitrile(B) at 0.20 mL/min.Samples were monitored via multiple reaction monitoring (MRM) model.External standard curve was used for quantitative analysis. The method exhibited a linear range of 0.5-10.0 μg/mL(r>0.99) for all compounds and the limits of detection(LOD) was 0.5μg/mL. The recoveries of GHB, 1,4-BD and GBL were 81.1%-87.7%, 98.5%-99.8% and 107.5%-116.2%, respectively, and relative standard derivation(RSD) ranges were 3.3%-5.7%, 3.7%-5.3% and 3.5%-5.1%(n=6), respectively. The RSD of accuracy, repeatability, stability and recovery of the method were all less than 6%(n=6). The method was sensitive, simple and rapid, and can be applied to the detection of target substances in different beverages.
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