摘要
目的:建立饮料中γ-羟基丁酸及其前体物质γ-丁内酯的超高效液相色谱-串级质谱(UPLC-MS/MS)定性定量检测方法。方法:样品经稀释后,选取Acquity UPLC HSS T3色谱柱(100 mm×2.1 mm,1.8μm)进行分离,以0.1%甲酸水溶液和甲醇作为流动相进行梯度洗脱,采用多反应监测模式(multiple reaction monitoring,MRM)进行分析。结果:γ-羟基丁酸在0.1-10μg·mL^-1浓度范围内线性关系良好,相关系数(r2)为0.998;γ-丁内酯在0.0226-2.26μg·mL-1浓度范围内线性关系良好,相关系数(r2)为0.997;γ-羟基丁酸的检出限10 ng·mL^-1,定量限25 ng·mL^-1;γ-丁内酯的检出限5 ng·mL^-1,定量限15 ng·mL^-1。γ-羟基丁酸和γ-丁内酯低中高3个浓度下的准确度为93%-110%,日内精密度RSD小于3.1%(n=6)。采用所建立的方法对2种8个批次的问题饮料进行分析,均准确测定样品中γ-羟基丁酸和γ-丁内酯的含量。结论:该方法样品处理简单,分析时间短,重复性和稳定性好,灵敏度高,准确可靠,适合于饮料中γ-羟基丁酸和γ-丁内酯的检测,并经过实际案件样品验证,定性定量结果和犯罪嫌疑人供述一致,具有司法实践意义。
Objective:To establish a method for qualitative and quantitative analysis ofγ-hydroxybutyric acid(GHB)andγ-butyrolactone(GBL)in beverages by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods:The sample was separated by Acquity UPLC HSS T3(100 mm×2.1 mm,1.8μm)column after dilution,and 0.1%formic acid water and methanol were used as mobile phase for gradient elution and then detected by UPLC-MS/MS.Results:The concentrations of GHB and GBL had a good linearity with the areas of peak in the range of 0.1-10μg·mL^-1and 0.0226-2.26μg·mL^-1,respectively.The correlation coefficients(r^2)were 0.998 and 0.997,respectively.The limit of detection and limit of quantification of GHB were10 ng·mL^-1and 25 ng·mL^-1,respectively.The limit of detection and limit of quantification of GBLwere 5 ng·mL^-1and 15 ng·mL^-1,respectively.The accuracies were 93%-110%,and the relative standard deviations(RSDs)were less than 3.1%(n=6).Conclusion:The method was simple,rapid,accurate and sensitive,and can meet the requirement for the determination of GHB and GBL in most of beverages.After actual case sample verification,qualitative and quantitative results are consistent with the confession of the criminal suspect,and is significant for judicial practice.
作者
陈月猛
钱振华
CHEN Yuemeng;QIAN Zhenhua(2.Institute of Forensic Science Ministry of Public Security People's Republic of China,Beijing,100038,China)
出处
《中国药物依赖性杂志》
CAS
CSCD
2019年第3期201-208,共8页
Chinese Journal of Drug Dependence
基金
中央级公益性科研院所基本科研业务费专项资金(2017JB030)
关键词
Γ-羟基丁酸
Γ-丁内酯
咔哇潮饮
咔哇氿
超高效液相色谱-串级质谱法
γ-hydroxybutyric acid
γ-butyrolactone
making wow drinks
making wow Gui
ultra performance liquid chromatography-tandem mass spectrometry