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,1.7μm),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(R 2>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.
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,1.7μm)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(R 2)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.
作者
方雅莉
马骥
FANG Yali;MA Ji(Scientific Research Platform Service Management Center,Guangdong Medical University,Dongguan 523000,China;Forensic Science Center,Dongguan Public Security Department,Dongguan 523000,China)
出处
《河北大学学报（自然科学版）》
CAS
北大核心
2023年第2期163-170,共8页
Journal of Hebei University(Natural Science Edition)
基金
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)。
