A high throughput screening method based on ultra performance liquid chromatogramphy-triple quadrupole composite linear ion trap mass spectrometry(UPLC-Q-TRAP/MS)was developed for the simultaneous and rapid confirmation of 49 common hypnotic and sedutive drugs. The pre-treatment method was based on solid-supported liquid liquid extraction(SLE). Waters C18 chromatographic column(2.1 mm×50 mm, 1.7 μm)was selected, with 0.1%(V/V)formic acid,5 mmoL/L ammonium acetate aqueous solution and methanol as mobile phases for gradient elution. The calibration curves showed good linearity in the range of 0.1~200.0 ng/mL,with correlation coefficients(R²)greater than 0.99 for all 49 analytes. The limits of highest detection and highest quantification of the 49 compounds were 0.1 ng/mL and 0.5 ng/mL, respectively. At spiked levels of 50、100、200 ng/mL, recoveries, intra-day precisions, and inter-day precisions of the 49 compounds were 65.9%~109.0%, 2.0%~17.6%, and 2.0%~16.3%, respectively. The established method is suitable for screening and testing these compounds in biological samples.- DOI:10.3969/j.issn.1000-1565.2023.02.008超高效液相色谱-三重四极杆串联质谱法检测全血中常见安眠镇静类药物方雅莉¹,马骥²(1.广东医科大学 科研平台服务管理中心,广东 东莞 523000;2.东莞市公安局 物证鉴定中心,广东 东莞 523000)摘 要:建立了超高效液相色谱-三重四极杆复合线性离子阱质谱快速筛查确证全血中49种安眠镇静类药物. 样品前处理采用固相支撑液液萃取法. 色谱条件:色谱柱为Waters C18(2.1 mm×50 mm,1.7 μm),以5 mmol/L乙酸铵-(体积分数为0.1%)甲酸水溶液(A),甲醇(B)为流动相,进行梯度洗脱. 在0.1~200.0 ng/mL内,49种常见药物展现出良好的线性关系(R²>0.99),最高检出限为0.1 ng/mL;最高定量限为0.5 ng/mL;全血基质中50、100、200 ng/mL 3个加标水平下回收率为65.9%~109.0%,日内精密度为2.0%~17.6%、日间精密度为2.0%~16.3%. 该方法可应用于生物检材中49种常见安眠镇静物质的检测.关键词:安眠镇静类药物;超高效液相色谱串联质谱;全血中图分类号:O657.7 文献标志码:A 文章编号:1000-1565(2023)02-0163-08Determination of common hypnotic and sedutive drugs in whole blood by UPLC-MS/MSFANG Yali¹, MA Ji²(1. Scientific Research Platform Service Management Center, Guangdong Medical University, Dongguan 523000, China; 2. Forensic Science Center, Dongguan Public Security Department, Dongguan 523000, China)Abstract: A high throughput screening method based on ultra performance liquid chromatogramphy-triple quadrupole composite linear ion trap mass spectrometry(UPLC-Q-TRAP/MS)was developed for the simultaneous and rapid confirmation of 49 common hypnotic and sedutive drugs. The pre-treatment method was based on solid-supported liquid liquid extraction(SLE). Waters C18 chromatographic column(2.1 mm×50 mm, 1.7 μm)was selected, with 0.1%(V/V)formic acid,5 mmoL/L ammonium acetate aqueous solution and methanol as mobile phases for gradient elution. The calibration curves showed good linearity in the range of 0.1~200.0 ng/mL,with correlation coefficients(R²)greater than 0.99 for all 49 analytes. The limits of highest detection and highest quantification of the 49 compounds were 0.1 ng/mL and 0.5 ng/mL, respectively. At spiked levels of 50、100、200 ng/mL, recoveries, intra-day precisions, and inter-day precisions of the 49 compounds were 65.9%~109.0%, 2.0%~17.6%, and 2.0%~16.3%, respectively. The established method is suitable for screening and testing these compounds in biological samples.- 收稿日期:2022-06-11 基金项目:广东医科大学青年培育基金自然科学类面上项目(GDMUQ2021050);广东省公安厅科技攻关项目(2022GDSSGG15;2022GDSSGG16) 第一作者:方雅莉(1991—),女,湖南岳阳人,广东医科大学实验师,主要从事化学分析和化学合成研究.E-mail:872173777@qq.com第2期方雅莉等:超高效液相色谱-三重四极杆串联质谱法检测全血中常见安眠镇静类药物河北大学学报(自然科学版) 第43卷