Gao Xue, Guo Hao, Du Yaoyu, Gu Chaokang
School of Environmental and Biological Engineering, Chongqing Technology and Business University, Chongqing 400067, China Chongqing Key Lab of Catalysis and Functional Organic Molecules, Chongqing Technology and Business University, Chongqing 400067, China.
Chongqing Institute of Forensic Science, Chongqing 400021, China
J Anal Toxicol. 2015 Jul-Aug;39(6):444-50. doi: 10.1093/jat/bkv040. Epub 2015 Apr 23.
Xylazine as veterinary medicine for sedation, but intoxication cases in humans were identified in the last few years. A highly sensitive method is required for analyzing xylazine and its metabolites in human blood and urine. This article presents an ultra high performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UHPLC-QTOF) study for simultaneous determination of xylazine and 2,6-dimethylaniline (DMA) in human blood and urine. The samples were extracted and cleaned up by Oasis MCX solid-phase extraction. The analysis is performed using an UHPLC-QTOF. Analysis precision, accuracy, sensitivity, linear range, limit of detection (LOD) and limit of quantification (LOQ) were validated for the proposed method. In the blood and urine samples, the linear calibration curves with high linearity are obtained over the range of 2.0-1,000.0 ng/mL. The LOD for xylazine and DMA in blood are 0.2 and 0.1 ng/mL, in urine are 0.4 and 0.2 ng/mL; the LOQ for xylazine and DMA in blood are 0.6 and 0.3 ng/mL, in urine are 1.0 and 0.6 ng/mL, respectively. The intra- and interday precision is better than 8.6 and 11.9%. In conclusion, the proposed method is highly sensitive and reproducible, thus suitable for accurate quantification of xylazine and its metabolites in blood and urine.
赛拉嗪作为兽用镇静剂，但在过去几年中发现了人类中毒病例。需要一种高灵敏度的方法来分析人血和尿液中的赛拉嗪及其代谢物。本文介绍了一种超高效液相色谱-四极杆飞行时间质谱联用（UHPLC-QTOF）研究，用于同时测定人血和尿液中的赛拉嗪和2,6-二甲基苯胺（DMA）。样品通过Oasis MCX固相萃取进行提取和净化。使用UHPLC-QTOF进行分析。对所提出的方法的分析精密度、准确度、灵敏度、线性范围、检测限（LOD）和定量限（LOQ）进行了验证。在血样和尿样中，在2.0-1000.0 ng/mL范围内获得了具有高线性的线性校准曲线。血样中赛拉嗪和DMA的LOD分别为0.2和0.1 ng/mL，尿样中分别为0.4和0.2 ng/mL；血样中赛拉嗪和DMA的LOQ分别为0.6和0.3 ng/mL，尿样中分别为1.0和0.6 ng/mL。日内和日间精密度分别优于8.6%和11.9%。总之，所提出的方法具有高灵敏度和重现性，因此适用于准确定量血样和尿样中的赛拉嗪及其代谢物。
