超高效液相色谱-串联质谱法检测唾液中3种毒品及其代谢物

建立了超高效液相色谱-串联质谱测定唾液中甲基苯丙胺、吗啡、O6-单乙酰吗啡等3种毒品及其代谢物的方法。以乙腈为提取液沉淀蛋白质法提取,采用基质提取溶液配制标准溶液制作定量曲线。采用BEH HILIC超高效液相色谱柱对待测毒品进行分离;采用电喷雾离子源正离子(ESI+)模式和多反应监测(MRM)模式进行质谱分析,以被测毒品的同位素内标进行定量。结果表明,在10、20、50、100 μg/L 4个添加水平下的回收率范围为(68.7±6.5)%～(110.8±4.6)%,日内精密度小于16.5%,日间精密度小于16.3%; 3种毒品的检出限(LOD,以信噪比(S/N)＞3计)和定量限(LOQ,以S/N＞10计)分别为0.02～0.05 μg/L和0.1～0.2 μg/L。方法快速、简便、定量准确、灵敏度高;在1 h之内即可对采集的唾液样品进行毒品定性和定量分析,可用于涉嫌吸毒者的快速认定。

Determination of three drugs and their metabolites in saliva by ultra performance liquid chromatography-tandem mass spectrometry

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method has been developed for the methamphetamine, morphine and O6-acetylmorphine in saliva. The sample was extracted and the protein was precipitated with acetonitrile. The matrix-matched standard solutions were used to prepare the curve of quantitative analysis. The drugs were separated on a BEH HILIC UPLC column. The mass spectrometric acquisition was carried out by means of electrospray ionization in positive mode (ESI+) with multiple reaction monitoring (MRM) method. The isotope internal standards were used to check the drugs. The average recoveries at four levels of 10, 20, 50 and 100 μg/L ranged from (68.7±6.5)% to (110.8±4.6)%. The intraday precisions were lower than 16.5% and interday precisions were lower than 16.3%. The detection limits (LOD, S/N＞3) and the quantification limits (LOQ, S/N＞10) of the three drugs were 0.02~0.05 μg/L and 0.1~0.2 μg/L, respectively. The saliva matrix effect was investigated. The method is rapid, simple, accurate and highly sensitive. The qualitative analysis and quantitative analysis of the collected saliva samples for the drugs can be finished within one hour, which is conducive to the rapid identification of the suspected drug addicts.