UHPLC-MS/MS Determination of 20 Common Drugs in Blood
摘 要
血液样品用乙腈提取,再以8 000 r·min-1转速离心10 min,取上清液,经0.22 μm有机滤膜过滤,采用超高效液相色谱-串联质谱法测定滤液中20种常见毒品的含量。以ACQUITY UPLC HSS C18色谱柱为固定相,以不同体积比的乙腈和pH 3.0的5 mmol·L-1甲酸铵溶液的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾正离子源和多反应监测模式。20种毒品的质量浓度均在10.0~100 μg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.10~5.00 μg·L-1。以空白样品为基体进行加标回收试验,所得回收率为42.3%~113%,测定值的日内相对标准偏差(n=5)为0.050%~15%,日间相对标准偏差(n=3)为2.1%~15%。
Abstract
The blood sample was extracted with acetonitrile, and then centrifugated for 10 min at the speed of 8 000 r·min-1. The supernatant was filtered on 0.22 μm organic filtration membrane. UHPLC-MS/MS was applied to the determination of 20 common drugs in the filtrate. ACQUITY UPLC HSS C18 chromatographic column was used as stationary phase, and the mixture of acetonitrile and 5 mmol·L-1 ammonium formate solution (pH 3.0) mixed in different ratios was used as mobile phase in gradient elution. ESI+ and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 20 drugs were kept in the same range of 10.0-100 μg·L-1, with detection limits (3S/N) in the range of 0.10-5.00 μg·L-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 42.3%-113%, with intra-day RSDs (n=5) and inter-day RSDs (n=3) of determined values in the ranges of 0.050%-15% and 2.1%-15%, respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201911005
所属栏目 工作简报
基金项目 中央级公益性科研院所基本科研业务费项目(2019JB042)
收稿日期 2019/4/19
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联系人作者王瑞花(nqkczs@126.com)
备注白利文,硕士研究生,研究方向为毒物毒品检验
引用该论文: BAI Liwen,WANG Aihua,YU Zhongshan,ZHANG Yuan,WANG Ruihua. UHPLC-MS/MS Determination of 20 Common Drugs in Blood[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(11): 1266~1273
白利文,王爱华,于忠山,张原,王瑞花. 超高效液相色谱-串联质谱法测定血液中20种常见毒品[J]. 理化检验-化学分册, 2019, 55(11): 1266~1273
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【3】张润生,王跨陡,龚飞君,等.苯丙胺类毒品及其衍生物的气相色谱-红外光谱分析[J].分析化学, 2012,40(6):915-919.
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【5】努尔艾力·塔依尔,毛新民,车文森,等.GC、GC-MS法定性定量法检测血液和尿液中阿片类毒品及其代谢物的含量[J].新疆医科大学学报, 2016,39(7):849-853.
【6】洪战英,吴玉田,吴侔天,等.GC/MS法检测头发中6-单乙酰吗啡和吗啡[J].药学学报, 1998,33(8):616-620.
【7】高凡钦,黄克建,李宏森,等.顶空固相微萃取与气质联用法同时快速检测尿样中14种常见滥用药物[J].分析试验室, 2014,33(5):604-608.
【8】黄爱芳,李建波,冯露敏,等.LC-MS法同时检测人血浆中杜冷丁、曲马多和美沙酮[J].中国卫生检验杂志, 2010,20(12):3191-3192.
【9】TIAN X, LIU B J, ZHANG Y H, et al. LC-MS/MS analysis and pharmacokinetics of sodium (±)-5-bromo-2-(α-hydroxypentyl) benzoate (BZP), an innovative potent anti-ischemic stroke agent in rats[J]. Molecules, 2016,21(4):501-512.
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【12】张睿,王海涛,吴斌,等.高效液相色谱-串联质谱法检测人血液中常见毒品残留量[J].分析试验室, 2011,30(10):71-74.
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