固相微萃取结合气质联用测定血浆中敌草快 |
| |
引用本文: | 高利娜,宋洋,祝娟,刘俊亭. 固相微萃取结合气质联用测定血浆中敌草快[J]. 中国法医学杂志, 2014, 0(5): 427-430 |
| |
作者姓名: | 高利娜 宋洋 祝娟 刘俊亭 |
| |
作者单位: | 中国医科大学药学院;中国医科大学法医学院; |
| |
摘 要: | 目的采用固相微萃取结合气相色谱-质谱联用方法快速测定血浆中的敌草快含量。方法采用硼氢化钠/氯化镍还原反应和顶空固相微萃取处理样本,气质联用检测方法,以乙基百草枯为内标,检测血浆中敌草快的含量,对还原反应和萃取的温度、时间等实验条件进行优化,并对方法学进行评价。结果采用m/z 194作为定性定量离子,在0.1~50μg/mL浓度范围内线性关系良好(Y=0.076 9X+0.274 8,r2=0.997 5),日内和日间精密度分别小于3.99%、5.64%。回收率为92.59%~101.27%,最低定量限为50ng/mL。敌草快还原产物1,1’-乙基-2,2’-联哌啶存在顺式和反式两种同分异构体,两者比率为1∶5.3,相对标准偏差为13.1%(n=17)。结论本文方法准确、快速、重现性好,可以在血浆等生物样品敌草快含量测定中选用。
|
关 键 词: | 法医毒物分析 敌草快 血浆 固相微萃取 气相色谱-质谱联用 同分异构体 |
Fast determination of diquat in plasma samples by solid phase microextraction combined with GC / MS |
| |
Affiliation: | Gao Lina, Song Yang, Zhu Juan, Liu Junting (1. School of Pharmacy, China Medical University, Shenyang 110001, China ; 2. School of Forensic Science, China Medical University, Shenyang 110001, China) |
| |
Abstract: | Objective We developed a method by GC/MS and headspace solid-phase microextraction (HS-SPME) for rapid determination of diquat in plasma samples. Methods The method involved the procedures of sodium borohydride-nickel chloride(NaBH4-NiCl2) reduction and HS-SPME. Ethyl-paraquat was used as internal standard. GC/MS was used to identify and quantify the analytes. The parameters that affected the reduction and extraction were also investigated, and the methodology was evaluated. Results In the range of 0. 1 -50 Ixg/mL, good linearity (Y = 0. 076 9X + 0. 274 8, r2 = 0. 997 5 ) was obtained using m/z 194 as quantifying ion. The intra- and inter-day precisions were less than 3.99%, 5.64%, respectively. Recoveries ranged from 92. 59% to 101.27%. LLOQ was 50ng/mL. We found that reduzates of diquat were cis-trans-isomer, and their peak area ratio was 1 : 5.3, with RSD% = 13.1% ( n = 17 ). Conclusion The method is sensitive, simple and rapid. It is recommendable for biological samples. |
| |
Keywords: | forensic toxicological analysis diquat plasma SPME GC/MS structural isomer |
本文献已被 CNKI 维普 等数据库收录! |
|