Department of Forensic Science, Fujian Police College, Fuzhou, China.
The Engineering Research Center, Fujian Police College, Fuzhou, China.
J Forensic Sci. 2021 Mar;66(2):748-757. doi: 10.1111/1556-4029.14624. Epub 2020 Dec 28.
With the rapid development of synthetic drugs, novel piperazine derivatives, as an increasingly important class of new psychoactive substances (NPS), have attracted global attention owing to their increasing demand in the illicit drug market. In this study, ten piperazine derivatives were analyzed in urine samples after pre-treatment with ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction (UA-LDS-DLLME) combined with gas chromatography-tandem mass spectrometry (GC-MS/MS). This simple approach involved the use of urine samples (1 mL) adjusted to pH 12, which was added to 100 µL of n-hexane and subjected to ultrasonication for 3 min to completely disperse the sample in the n-hexane solution. The resulting turbid suspension was centrifuged at 10,000 rpm for 3 min, and the supernatant was extracted and analyzed using GC-MS/MS. Under the optimized conditions presented in this study, the linear relationship between the analytes was good within 10-1500 ng/mL, and the correlation coefficient (r) was between .9914 and .9983. The limit of detection (LOD) was 0.3-2 ng/mL (S/N = 3), and the lower limit of quantification (LLOQ) was 10 ng/mL (S/N = 10) with the recovery of the analytes of interest from the spiked samples being 76.3%-93.3%. This method has been used to analyze real-world samples; our study shows that the UA-LDS-DLLME approach can be used for rapid analysis while consuming minimal solvent for the simultaneous determination of a range of analytes. This method has the potential for use in clinical analyses and forensic toxicology.
随着合成毒品的迅速发展，新型哌嗪衍生物作为越来越重要的一类新型精神活性物质（NPS），由于其在非法毒品市场的需求不断增加，引起了全球关注。在这项研究中，采用超声辅助低密度溶剂分散液液微萃取（UA-LDS-DLLME）与气相色谱-串联质谱（GC-MS/MS）相结合的方法，对尿液样品中的 10 种哌嗪衍生物进行了分析。该方法操作简单，使用 pH 值为 12 的尿液样品（1 mL），加入 100 µL 正己烷，超声 3 分钟，使样品完全分散在正己烷溶液中。将得到的混浊悬浮液以 10,000 rpm 的速度离心 3 分钟，提取上清液并使用 GC-MS/MS 进行分析。在本研究中提出的优化条件下，分析物的线性关系良好，在 10-1500ng/mL 范围内，相关系数（r）在.9914 至.9983 之间。检出限（LOD）为 0.3-2ng/mL（S/N=3），定量下限（LLOQ）为 10ng/mL（S/N=10），感兴趣分析物在加标样品中的回收率为 76.3%-93.3%。该方法已用于分析实际样品；我们的研究表明，UA-LDS-DLLME 方法可以用于快速分析，同时消耗最少的溶剂，用于同时测定一系列分析物。该方法有望用于临床分析和法医毒理学。
