LTQ-Orbitrap组合式高分辨质谱法快速筛查毛发中7种毒品及代谢物

摘要

A new method was developed for the determination of seven illicit drugs and metabolites in human hair by ultra high performance liquid chromatograph tandem a linear ion trap-orbitrap hybrid instrument at high mass resolution (UHPLC-LTQ-Orbitrap/MS). After being washed and grinded, the hair samples were soaked in pH 9. 2 borate buffer with ultrasonic for 90 min. Then the samples were extracted by solid phase extraction (SPE). High resolution mass spectrometry was applied to reduce matrix interference. Full scanning of electrostatic field orbitrap was applied for quantification of drugs. The limits of detection (LOD) of seven illicit drugs and metabolites in human hair were 0. 001 -0. 02 μg/g. The method showed a fairly good linearity over the range of 0. 05 - 50 μg/g (r>0. 9975). The spiked recoveries were between 76. 1% -109. 6% , and the deviation of intra- and inter- day precision was less than 14. 9%. The method is simple, high sensitive, and suitable for the determination of illicit drugs in human hair.%采用超高压液相色谱-二维线性离子阱结合静电场轨道阱组合式高分辨质谱联用技术(Accela U-HPLC/LTQ Orbitrap XL),建立了人毛发中吗啡、O6-单乙酰吗啡、可待因、乙酰可待因、氯胺酮、去甲氯胺酮和美沙酮毒品及代谢物快速筛查方法.取毛发样品经表层清洗后冷冻研磨粉碎,置于硼酸盐缓冲液(pH 9.2)中超声90 min,离心取上清液,用Oasis HLB柱固相萃取制备.通过静电场轨道阱全扫描得到毒品及其代谢物的精确相对分子质量,同时进行7种毒品及其代谢物的快速筛查.高分辨率质谱可有效去除毛发基质干扰,毒品及其代谢物筛查检出限在0.001～0.02 ng/mg,在0.05～50 ng/mg范围内存在良好线性关系(r＞0.9975)；本方法平均加标回收率为76.1％～109.6％；日内及日间精密度RSD≤14.9％.本方法灵敏度高,样品制备简便,适用于常见毒品的快速筛查.