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QuEChERS-超高效液相色谱-质谱联用法检测小鼠血中5种尼秦类新精神活性物质
Determination of five new psychoactive nitazenes in blood of mice by QuEChERS combined with UPLC-MS/MS
【摘要】 目的:建立了基于QuEChERS前处理技术同时测定小鼠血中5种尼秦类物质的超高效液相色谱-串联质谱法(UPLC-MS/MS)。方法:样本采用甲醇:乙腈(1∶3,体积比)提取,MgSO4脱水,以XSelect HSS T3色谱柱(2.1 mm×100 mm)进行色谱分离,正离子多反应监测(MRM)模式检测,以甲醇-0.1%甲酸水为流动相进行梯度洗脱。结果:血中5种尼秦类物质在0.1~100 ng·m L-1范围内线性关系良好,相关系数均> 0.999 0。方法检出限为0.4~2.0 pg·m L-1,定量下限为1.3~6.3 pg·m L-1,加标回收率(n=6)为89.4%~110%,相对标准偏差(RSD)为3.9%~6.3%。结论:该方法具有灵敏、准确、操作性强的优点,可用于血液中5种尼秦类物质的检验,为涉毒案件提供科学依据。
【Abstract】 Objective: A method was established for the simultaneous determination of five nitazenes in the blood of mice using ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) based on Qu ECh ERS pretreatment technology. Methods: The samples were extracted with a mixture of methanol-acetonitrile(1 ∶ 3, volume ratio) and dehydrated with MgSO4. The samples were separated on an XSelect HSS T3 column(2.1 mm×100 mm) by positive ion scanning in multiple reaction monitoring(MRM) mode, with gradient elution using a mobile phase composed of methanol-0.1% formic acid aqueous solution. Results: Five nitazenes exhibited good linearities within the concentration range of 0.1-100 ng · mL-1, with correlation coefficients all exceeding 0.999 0. The limits of detection(LOD) of five nitazenes were within the range of 0.4-2.0 pg · m L-1, and the limits of quantitation(LOQ) were within the range of 1.3-6.3 pg · m L-1. The spiked recovery rates(n=6) ranged from 89.4% to 110%, with relative standard deviations(RSD) of 3.9%-6.3%. Conclusion: This method offers advantages including high sensitivity, accuracy, and strong operability. It can be effectively applied to detect five nitazenes in blood samples, providing a scientific basis for drug-related cases.
【Key words】 ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS); metonitazene; N-desethyl etonitazene; N-desethyl isotonitazene; etonitazepyne; protonitazepyne; blood of mice; QuEChERS(quick,easy,cheap,effective,rugged,safe);
- 【文献出处】 药物分析杂志 ,Chinese Journal of Pharmaceutical Analysis , 编辑部邮箱 ,2026年02期
- 【分类号】R965;O657.63
- 【下载频次】71