Servicio de Toxicología Forense, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, San Francisco s/n, 15782 Santiago de Compostela, Spain.
J Chromatogr A. 2013 Jun 21;1295:99-106. doi: 10.1016/j.chroma.2013.04.035. Epub 2013 Apr 22.
An LC-MS/MS method for the quantification of the synthetic cannabinoids JWH-200, JWH-250, JWH-073, JWH-018, HU-211, CP 47,497 and CP 47,497-C8, and THC in oral fluid was developed and validated. Samples (0.5 mL) were extracted using Strata X cartridges (Phenomenex). Chromatographic separation was achieved with a Sunfire™ IS column (20×2.1 mm, 3.5 μm) (Waters Corp.), with formic acid 0.1% and acetonitrile as mobile phase. A different chromatographic gradient was applied for the separation of the analytes depending on the ionization mode employed, with a total chromatographic run of 14 min. Detection was performed in a Quattro Micro™ API ESCI (Waters Corp.), using electrospray in the positive mode (ESI+) for JWH-200, JWH-250, JWH-073, JWH-018 and THC, and ESI- for HU-211, CP 47,497, and CP 47,497-C8. Validation of the method included the assessment of selectivity, linearity (0.1-2.5 to 200 ng/mL), limits of detection (0.025-1 ng/mL) and quantification (0.1-2.5 ng/mL), imprecision (%CV≤14.4%), accuracy (91.8-109.7% of target concentration), extraction recovery (65.4-105.6%) and Quantisal recovery (56.1-66.7%), and matrix effect (neat oral fluid: -56.0% to 38.5%; oral fluid in Quantisal buffer: -15.1% to -71.7%). The application of this method to oral fluid samples from roadside testing will provide unique information on the use of these new synthetic drugs by Spanish drivers.
建立并验证了一种 LC-MS/MS 方法,用于对唾液中的合成大麻素 JWH-200、JWH-250、JWH-073、JWH-018、HU-211、CP 47,497 和 CP 47,497-C8 以及四氢大麻酚进行定量分析。样品(0.5mL)经 Strata X 萃取柱(Phenomenex)萃取。采用 Sunfire™ IS 柱(20×2.1mm,3.5μm)(Waters Corp.)进行色谱分离,流动相为甲酸 0.1%和乙腈。根据所采用的电离模式,采用不同的色谱梯度对分析物进行分离,总色谱运行时间为 14 分钟。检测采用 Quattro Micro™ API ESCI(Waters Corp.),JWH-200、JWH-250、JWH-073、JWH-018 和四氢大麻酚采用正电喷雾(ESI+)模式进行电喷雾,HU-211、CP 47,497 和 CP 47,497-C8 则采用电喷雾(ESI-)模式进行检测。方法验证包括选择性、线性(0.1-2.5 至 200ng/mL)、检测限(0.025-1ng/mL)和定量限(0.1-2.5ng/mL)、精密度(%CV≤14.4%)、准确度(目标浓度的 91.8-109.7%)、提取回收率(65.4-105.6%)和 Quantisal 回收率(56.1-66.7%)以及基质效应(未稀释的唾液:-56.0%至 38.5%;Quantisal 缓冲液中的唾液:-15.1%至-71.7%)。该方法应用于路边检测的唾液样品,将为西班牙驾驶员使用这些新型合成药物提供独特的信息。