The State Laboratory, Backweston Laboratory Complex, Young's Cross, Celbridge, Co. Kildare, Ireland.
J Chromatogr A. 2010 Oct 29;1217(44):6857-66. doi: 10.1016/j.chroma.2010.08.043. Epub 2010 Sep 18.
A rapid method has been developed to analyse morphine, codeine, morphine-3-glucuronide, 6-monoacetylmorphine, cocaine, benzoylegonine, buprenorphine, dihydrocodeine, cocaethylene, 3,4-methylenedioxyamphetamine, ketamine, 3,4-methylenedioxymethamphetamine, pseudoephedrine, lignocaine, benzylpiperazine, methamphetamine, amphetamine, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine and methadone in human urine. Urine samples were diluted with methanol:water (1:1, v/v) and sample aliquots were analysed by hybrid linear ion trap-triple quadrupole mass spectrometry with a runtime of 12.5 min. Multiple reaction monitoring (MRM) as survey scan and an enhanced product ion (EPI) scan as dependent scan were performed in an information-dependent acquisition (IDA) experiment. Finally, drug identification and confirmation was carried out by library search with a developed in-house MS/MS library based on EPI spectra at a collision energy spread of 35±15 in positive mode and MRM ratios. The method was validated in urine, according to the criteria defined in Commission Decision 2002/657/EC. At least two MRM transitions for each substance were monitored in addition to EPI spectra and deuterated analytes were used as internal standards for quantitation. The reporting level was 0.05 μg mL(-1) for the range of analytes tested. The regression coefficients (r(2)) for the calibration curves (0-4 μg mL(-1)) in the study were ≥0.98. The method proved to be simple and time efficient and was implemented as an analytical strategy for the illicit drug monitoring of opioids, cocaines and amphetamines in criminal samples from crime offenders, abusers or victims in the Republic of Ireland. To the best of our knowledge there are no hybrid LC-MS applications using MRM mode and product ion spectra in the linear ion trap mode for opioids, cocaines or amphetamines with validation data in urine.
已经开发出一种快速方法来分析吗啡、可待因、吗啡-3-葡糖苷酸、6-单乙酰吗啡、可卡因、苯甲酰海洛因、丁丙诺啡、二氢可待因、古柯乙醇、3,4-亚甲二氧基苯丙胺、氯胺酮、3,4-亚甲二氧基甲基苯丙胺、伪麻黄碱、利多卡因、苄基哌嗪、甲基苯丙胺、苯丙胺、2-亚乙基-1,5-二甲基-3,3-二苯基吡咯烷和美沙酮在人尿中的含量。尿样用甲醇：水（1:1，v/v）稀释，样品等分试样用混合线性离子阱-三重四极杆质谱仪分析，运行时间为 12.5 分钟。多重反应监测（MRM）作为综述扫描，增强产物离子（EPI）扫描作为依赖扫描，在信息依赖性采集（IDA）实验中进行。最后，通过基于 EPI 谱在正模式下碰撞能展宽 35±15 的内部 MS/MS 库进行库搜索进行药物鉴定和确认。该方法根据委员会 2002/657/EC 号决定的标准在尿液中进行了验证。除了 EPI 谱外，还监测了每种物质的至少两个 MRM 转换，并用氘代分析物作为定量的内标。检测限为 0.05μg/mL，用于测试的分析物范围。研究中校准曲线（0-4μg/mL）的回归系数（r(2)）≥0.98。该方法简单、高效，已作为分析策略应用于爱尔兰共和国犯罪样本中来自犯罪者、滥用者或受害者的阿片类药物、可卡因和苯丙胺的非法药物监测。据我们所知，没有使用 MRM 模式和线性离子阱模式下的产物离子谱对阿片类药物、可卡因或苯丙胺进行 LC-MS 混合应用，并在尿液中提供验证数据。
