Ji Jiao-Jiao, Yan Hui, Xiang Ping, Shen Baohua, Shen Min
Department of Forensic Toxicology, Shanghai Key Laboratory of Forensic Medicine, Academy of Forensic Science, Shanghai 200063, China; East China University of Political Science and Law, Shanghai 200042, China.
Department of Forensic Toxicology, Shanghai Key Laboratory of Forensic Medicine, Academy of Forensic Science, Shanghai 200063, China.
Forensic Sci Int. 2019 Aug;301:341-349. doi: 10.1016/j.forsciint.2019.05.040. Epub 2019 May 24.
A rapid, sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination and quantification of 12 psychotropic drugs and metabolites in hair was developed and validated. After freeze grinding with methanol, the supernatant was determined by LC-MS/MS using an Allure PFPPropyl column (100 × 2.1 mm, 5 μm) with a gradient elution of acetonitrile and 10 mmol/L ammonium acetate with 0.1% formic acid, and in the subsequent analysis using multiple reaction monitoring (MRM) mode, two ion transitions were monitored for each analyte. The limits of detection ranged from 0.002 to 0.05 ng/mg, and the limits of quantitation were in the range of 0.005-0.1 ng/mg. Good linearity (r > 0.995) was observed for all analytes over the linear range. Acceptable intraday and interday precision (RSD ≤ 20%) and accuracy (85.3%-112.9%) were achieved. This method of detection was applied to the analysis of guinea pig hair roots after a single dose of quetiapine. Quetiapine and 7-hydroxyquetiapine were both detected in guinea pig hair roots from 5 min post administration. The concentration of quetiapine (10.3-1733.8 ng/mg) was much higher than that of 7-hydroxyquetiapine (0.1-40.6 ng/mg) in the hair roots of guinea pigs, and higher concentrations of quetiapine and 7-hydroxyquetiapine occurred in black hair root than in that of white and brown. The animal experiment demonstrated that hair roots may be a good specimen for proving acute quetiapine poisoning when other biological matrices are not available.
建立并验证了一种快速、灵敏的液相色谱-串联质谱（LC-MS/MS）法，用于测定和定量毛发中的12种精神药物及其代谢物。用甲醇冷冻研磨后，取上清液通过LC-MS/MS测定，采用Allure PFP丙基柱（100×2.1 mm，5μm），以乙腈和含0.1%甲酸的10 mmol/L醋酸铵进行梯度洗脱，在随后的多反应监测（MRM）模式分析中，对每种分析物监测两个离子跃迁。检测限为0.002至0.05 ng/mg，定量限为0.005 - 0.1 ng/mg。所有分析物在线性范围内均呈现良好的线性（r＞0.995）。获得了可接受的日内和日间精密度（RSD≤20%）和准确度（85.3% - 112.9%）。该检测方法应用于单次服用喹硫平后豚鼠毛根的分析。给药后5分钟，在豚鼠毛根中检测到喹硫平和7-羟基喹硫平。豚鼠毛根中喹硫平的浓度（10.3 - 1733.8 ng/mg）远高于7-羟基喹硫平（0.1 - 40.6 ng/mg），且黑色毛根中喹硫平和7-羟基喹硫平的浓度高于白色和棕色毛根。动物实验表明，当没有其他生物基质时，毛根可能是证明急性喹硫平中毒的良好标本。
