LC-MS/MS分析生物检材中的呋喃酚葡萄糖醛酸结合物  

Analyzing intact carbofuran-7-phenyl glucuronic acid in biological samples by LC-MS/MS

作　　者：王颖 赵辛[2] 路玉平 贾娟[1] 马红娟 傅善林 刘耀[1,4] 丛斌[1,5] David Richard Fowler 尉志文[1] 贠克明[1] Wang Ying;Zhao Xin;Lu Yuping;Jia Juan;Ma Hongjuan;Fu Shanlin;Liu Yao;Cong Bin;David Richard Fowler;Wei Zhiwen;Yun Keming(School of Forensic Medicine,Shanxi Medical University,Taiyuan 030001,Shanxi,China;Jiancaoping Branch of the Taiyuan Public Security Bureau,Taiyuan 030023,Shanxi,China;Centre for Forensic Science,University of Technology,Sydney 2007,Australia;Institute of Forensic Science,The Ministry of Public Security,Beijing 100038,China;School of Forensic Medicine,Hebei Medical University,Shijiazhuang 050017,Hebei,China;University of Maryland,Baltimore,Maryland,21201,USA)

机构地区：[1]山西医科大学法医学院,山西太原030001 [2]太原市公安局,山西太原030001 [3]澳大利亚悉尼科技大学法庭科学研究中心,澳大利亚悉尼NSW 2007 [4]公安部物证鉴定中心,北京100038 [5]河北医科大学法医学系,河北石家庄050017 [6]美国马里兰大学,美国马里兰州巴尔地摩21201

出　　处：《中国法医学杂志》2020年第4期380-384,共5页Chinese Journal of Forensic Medicine

基　　金：国家重点研发计划课题项目资助(2017YFC0803504,2018YFC0807403);国家科技基础专项项目资助(SQ2015FY111400)。

摘　　要：目的建立生物检材中呋喃酚葡萄糖醛酸结合物的LC-MS/MS检测方法。方法血和肝等检材经乙腈沉淀蛋白,采用ZORBAX HILIC Plus(4.6mm×100mm,3.5μm)亲水性色谱柱,以水和含0.1%甲酸的乙腈为流动相,梯度洗脱,以负离子多反应检测(MRM)模式检测,扫描时间8min。结果血和肝中呋喃酚葡萄糖醛酸结合物的线性范围分别是20ng/ml^5μg/ml和50ng/g^5μg/g,线性关系良好,r^2均大于0.999,血和肝中最低检出限分别为10ng/ml和9.93ng/g,最低定量限分别为15.63ng/ml和16.56ng/g;批内及批间精密度分别在1.53%~5.02%和5.06%~6.85%;相对回收率为86.13%~92.71%和87.01%~94.06%。对一例克百威中毒死亡人体检材进行检测,克百威及呋喃酚的血浓度分别为0.77ug/g和29.65ug/g,呋喃酚葡萄糖醛酸结合物的血浓度为1.059ug/g,肝组织浓度为4.056 ug/g。结论本研究所建方法特异性强、灵敏度高,可满足法医学中对于血中呋喃酚葡萄糖醛酸结合物的检测需求。Objective To establish a detection method of intact carbofuran-7-phenyl glucuronic acid in biological samples by LC-MS/MS. Method Blood and liver samples were precipitated with acetonitrile. ZORBAX HILIC Plus(4.6×100 mm, 3.5 μm), a hydrophilic column, was used to analyze. The mobile phases were water and 0.1% formic acid in acetonitrile, gradient elution. Then the eluant was detected in multiple reaction monitoring(MRM) mode with negative ionization, scanning for 8 min. Results The linear range of carbofuran-7-phenyl glucuronic acid in the blood and liver is 20 ng/ml^5 ug/ml and 50 ng/g^5 ug/g, respectively and the linear relationship is good. Regression coefficient R is greater than 0.999, and the minimum limit of detection in blood and liver is 10 ng/ml and 9.93 ng/ml, respectively, the minimum limit of quantification is 15.63 ng/ml and 16.56 ng/g, respectively;the intra-assay and inter-assay precision are 1.53%~5.02% and 5.06%~6.85%;the relative recovery rate is 86.13%~92.71% and 87.01%~94.06%. A case of carbofuran poisoning is analyzed, the blood content of carbofuran and carbofuran-phenol is 0.77 ug/ml and 29. 65 ug/ml. The concentration of carbofuran-7-phenyl glucuronic acid in blood is 1.059 ug/ml, while in the liver is 4.056 ug/g. Conclusion The method can meet the requirements of analyzing carbofuran-7-phenyl glucuronic acid in biological samples, due to its high specificity and sensitivity.

关 键 词：法医毒物分析 克百威 液相色谱-串联质谱 呋喃酚葡萄糖醛酸结合物 生物检材 

分 类 号：DF795.1[医药卫生—法医学]