Liu Hsiu-Chuan, Lee Hsi-Tzu, Hsu Ya-Ching, Huang Mei-Han, Liu Ray H, Chen Tai-Jui, Lin Dong-Liang
Department of Forensic Toxicology, Institute of Forensic Medicine, Ministry of Justice, Taipei, Taiwan.
Department of Medical Laboratory Science and Biotechnology, Fooyin University, Kaohsiung, Taiwan.
J Anal Toxicol. 2015 Jul-Aug;39(6):472-80. doi: 10.1093/jat/bkv041. Epub 2015 May 2.
A rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS-MS) method was developed, validated and applied to simultaneous analysis of oral fluid samples for the following 10 analytes: methadone, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP), buprenorphine, norbuprenorphine, morphine, codeine, 6-acetylmorphine, 6-acetylcodeine, amphetamine, and methamphetamine. The oral fluid sample was briefly centrifuged and the supernatant was directly injected into the LC-MS-MS system operated under reverse-phase chromatography and electrospray ionization (ESI). Deuterated analogs of the analytes were adopted as the internal standards and found to be effective (except for buprenorphine) to compensate for potential matrix effects. Each analytical run took <10 min. Linearity range (r(2) > 0.99) established for buprenorphine and the other nine analytes were 5-100 and 1-100 ng/mL. Intra- and interday precision (% CV) ranges for the 10 analytes were 0.87-12.2% and 1.27-12.8%, while the corresponding accuracy (%) ranges were 91.8-113% and 91.9-111%. Limits of detection and quantitation established for these 10 analytes were in the ranges of 0.1-1.0 and 0.25-1.0 ng/mL (5 ng/mL for buprenorphine). The method was successfully applied to the analysis of 62 oral fluid specimens collected from patients participating in methadone and buprenorphine substitution therapy programs. Analytical results of methadone and buprenorphine were compared with data derived from GC-MS analysis and found to be compatible. Overall, the direct injection LC-MS-MS method performed well, permitting rapid analysis of oral fluid samples for simultaneous quantification of methadone, buprenorphine, opiate and amphetamine drug categories without extensive sample preparation steps.
建立了一种快速灵敏的液相色谱 - 串联质谱(LC-MS-MS)方法,并进行了验证,该方法用于同时分析口腔液样本中的以下10种分析物:美沙酮、2-亚乙基-1,5-二甲基-3,3-二苯基吡咯烷(EDDP)、丁丙诺啡、去甲丁丙诺啡、吗啡、可待因、6-乙酰吗啡、6-乙酰可待因、苯丙胺和甲基苯丙胺。口腔液样本经短暂离心后,上清液直接注入在反相色谱和电喷雾电离(ESI)条件下运行的LC-MS-MS系统。分析物的氘代类似物用作内标,发现其可有效(丁丙诺啡除外)补偿潜在的基质效应。每次分析运行时间<10分钟。丁丙诺啡及其他9种分析物的线性范围(r(2)>0.99)分别为5-100和1-100 ng/mL。10种分析物的日内和日间精密度(%CV)范围分别为0.87-12.2%和1.27-12.8%,相应的准确度(%)范围分别为91.8-113%和91.9-111%。这10种分析物的检测限和定量限范围分别为0.1-1.0和0.25-1.0 ng/mL(丁丙诺啡为5 ng/mL)。该方法成功应用于分析从参与美沙酮和丁丙诺啡替代治疗项目的患者中收集的62份口腔液标本。将美沙酮和丁丙诺啡的分析结果与气相色谱 - 质谱(GC-MS)分析数据进行比较,发现结果相符。总体而言,直接进样LC-MS-MS方法性能良好,无需大量样本制备步骤即可快速分析口腔液样本,同时定量美沙酮、丁丙诺啡、阿片类药物和苯丙胺类药物。