UPLC-MS/MS快速测定血液中布桂嗪  

Rapid Determination of Bucinnazine in Blood by UPLC-MS/MS

作　　者：高章明 石景瑜 曾皓 张学军 GAO Zhang-ming;SHI Jing-yu;ZENG Hao;ZHANG Xue-jun(Institute of Forensic Science,Shangrao Public Security Bureau,Shangrao 334000,Jiangxi Province,China;Pharmacy Department of Shangrao Guangxin District People’s Hospital,Shangrao 334100,Jiangxi Province,China;Drug Testing Center of Jiangxi Provincial Public Security Department,Nanchang 330000,China)

机构地区：[1]上饶市公安局物证鉴定中心,江西上饶334000 [2]上饶市广信区人民医院药剂科,江西上饶334100 [3]江西省公安厅毒品检验鉴定中心,江西南昌330000

出　　处：《法医学杂志》2023年第4期388-392,共5页Journal of Forensic Medicine

摘　　要：目的建立血液中布桂嗪的UPLC-MS/MS快速分析方法,并应用于实际案例。方法血液中加入内标后,用900μL混合溶液(V_(乙腈)∶V_(水)=8∶2)沉淀蛋白,涡旋离心后,过0.22μm滤膜后测定。经C18色谱柱分离,以乙腈和5 mmol/L乙酸铵水溶液(含0.1%甲酸)为流动相梯度洗脱,流速0.4 mL/min,电喷雾正离子模式下进行多反应监测扫描,内标法定量,并进行方法学验证。结果血液中布桂嗪在0.5~200μg/L范围线性关系良好,相关系数(r)为0.9997,检出限为0.1μg/L,定量限为0.5μg/L,在1、10、100μg/L3个质量浓度水平的回收率为78.3%~83.8%,基质效应为69.4%~73.8%,日内精密度为1.9%~2.8%,日间精密度为2.8%~3.2%,准确度为3.1%~3.5%。-25℃下1、100μg/L两个质量浓度的稳定性实验结果显示,10 d准确度(偏倚)≤4.5%。结论本方法前处理过程简单,样品处理速度快,仪器分析灵敏度高,含量测定稳定性好,鉴定结果可靠,可满足案件鉴定的需要。Objective To establish a rapid method for the analysis of bucinnazine in blood by UPLCMS/MS and to apply the method to the practical case.Methods After the internal standard was added to blood,the protein was precipitated with 900μL mixed solution(V_(acetonitrile)∶V_(water)=8∶2).After vortex and centrifugation,the protein was measured through 0.22μm filter membrane.The separation was performed on C18 chromatography column,with acetonitrile and 5 mmol/L ammonium acetate containing 0.1% formic acid aqueous as mobile phase gradient elution at the flow rate of 0.4 mL/min.Multiple reaction monitoring scan was performed in electrospray positive ion mode,quantitative measurement was performed by internal standard method,and methodological verification was carried out.Results The linear relationship of bucinnazine in blood was good in the range of 0.5-200μg/L,the correlation coefficient(r)was 0.9997,the limit of detection was 0.1μg/L,the limit of quantitation was 0.5μg/L,and the recovery was 78.3%-83.8% at 1,10 and 100μg/L mass concentration levels.The matrix effect was 69.4%-73.8%,the intra-day precision was 1.9%-2.8%,and the inter-day precision was 2.8%-3.2%,the accuracy was 3.1%-3.5%.The stability test results of 1 and 100μg/L mass concentrations at -25℃ showed that the accuracy(bias)of 10 d was less than 4.5%.Conclusion This method has the advantages of simple pre-treatment process,fast sample processing speed,high sensitivity of instrument analysis,good stability of content determination and reliable identification results,and can meet the needs of case identification.

关 键 词：法医学 毒物分析 布桂嗪 血液 超高效液相色谱-串联质谱法 

分 类 号：R89[医药卫生—法医学] DF795.1[医药卫生—临床医学] D919.1[政治法律—诉讼法学]