Department of Forensic Toxicology, Shanghai Key Laboratory of Forensic Medicine, Shanghai Forensic Science Platform, Academy of Forensic Science, Shanghai, 200063, China.
School of Pharmacy, Guangdong Pharmaceutical University, Guangzhou, 510006, China.
Sci Rep. 2020 Jul 14;10(1):11569. doi: 10.1038/s41598-020-68348-w.
The recent emergence of new fentanyl analogues and synthetic opioids on the drug market poses a global public health threat. However, these compounds cannot typically be identified using existing analytical methods. In this study, we aimed to develop and validate a rapid and sensitive method based on ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for the simultaneous determination of 37 fentanyl analogues and novel synthetic opioids in hair samples. Hair samples (20 mg) were extracted by cryogenic grinding in an extraction medium of methanol, acetonitrile, and 2 mmol/L ammonium acetate (pH 5.3). Following centrifugation of the samples, the analytes were separated using a WATERS Acquity UPLC HSS T column. The limits of detection (LODs) and limits of quantification (LOQs) ranged from 0.5 to 2.5 pg/mg and from 2 to 5 pg/mg, respectively. The intraday and interday precisions were within 13.32% at LOQ, low, medium, and high levels. The accuracies were within the range of 85.63-116.1%. The extraction recoveries were in the range of 89.42-119.68%, and the matrix effects were within the range of 44.81-119.77%. Furthermore, the method was successfully applied to the detection and quantification of fentanyl and sufentanil in hair samples from two authentic cases. Thus, this method has great potential for detecting fentanyl analogues and novel synthetic opioids in forensic work.
新芬太尼类似物和合成阿片类药物在毒品市场上的出现,对全球公共卫生构成了威胁。然而,这些化合物通常无法使用现有的分析方法来识别。在本研究中,我们旨在开发和验证一种基于超高效液相色谱-串联质谱(UHPLC-MS/MS)的快速灵敏方法,用于同时测定头发样品中 37 种芬太尼类似物和新型合成阿片类药物。头发样品(20mg)用甲醇、乙腈和 2mmol/L 乙酸铵(pH5.3)的提取介质在低温研磨下提取。样品离心后,用沃特世 Acquity UPLC HSS T 柱分离分析物。检出限(LOD)和定量限(LOQ)范围分别为 0.5-2.5pg/mg 和 2-5pg/mg。在 LOQ、低、中、高水平下,日内和日间精密度均在 13.32%以内。准确度在 85.63-116.1%范围内。提取回收率在 89.42-119.68%范围内,基质效应在 44.81-119.77%范围内。此外,该方法成功应用于两个真实案例中头发样品中芬太尼和舒芬太尼的检测和定量。因此,该方法在法医工作中检测芬太尼类似物和新型合成阿片类药物具有很大的潜力。