LC-MS/MS同时分析尿液中15种安眠镇静药物及其代谢物

目的建立尿液中15种常见安眠镇静药物及代谢物的液相色谱-串联质谱分析方法。方法尿液经酶水解、固相萃取后,用C18液相柱分离,以含甲酸铵和甲酸的水、乙腈为流动相梯度洗脱,质谱采用电喷雾电离（ESI）-正负离子模式同时扫描,采用二级质谱多反应监测（MRM）模式检测目标化合物。结果以化合物的保留时间、两对母离子/子离子对定性,尿中常见安眠镇静药物的检测限为0.01～0.5ng/mL（ESI＋）和10ng/mL（ESI-）;相关系数r在0.994以上;日内及日间精密度均在18%以下;绝对回收率在64.80%～116.20%之间。结论方法快速、灵敏、简便、可靠,能同时分析尿液中的15种安眠镇静药物及其代谢物。

Simultaneous Analysis of 15 Sedative-hypnotics and Their Metabolites in Urine by LC-MS/MS

Objective To establish a liquid chromatography-tandem mass spectrum （LC-MS/MS） method for simultaneous analysis of 15 sedative-hypnotics and some metabolites in urine samples. Methods Urine samples were enzyme-hydrolyzed and extracted by solid phase extraction （SPE）, then separated by C18 column and analyzed by MS. The positive and negative electric spray ionization modes were adopted simultaneously. Multiple reaction monitoring （MRM） mode was used to analyze target compounds. Results Identification was based on the compound＇s retention time and two pairs of precursor-to-product ion transitions. The limits of detection （LOD） ranged from 0.01ng/mL to 0.5ng/mL（ESI＋） and lOng/mL （ESI-） in urine, and showed a fairly good linearity over the range of 2-3 orders （r〉0.994）. The recovery rates were between 64.80% - 116.20%, and the deviation of intra- and inter-day precision was less than 18%. Conclusion This newly developed method shows high sensitivity and selectivity, and is suitable for the simultaneous analysis of 15 sedative-hypnotics and some metabolites in urine samples.