法医学杂志

法医学杂志 ›› 2008, Vol. 0 ›› Issue (6): 429-432.

• 论文 • 上一篇    下一篇

硼氢化钠/氯化镍还原-GC/TSD法检测血液和尿液中百草枯

黄璐瑶;廖林川;陈礼莉;粟贵;李雯佳;何荣;颜有仪;杨林;   

  1. 四川大学华西基础医学与法医学院;四川大学华西药学院;
  • 发布日期:2008-12-25 出版日期:2008-12-28

Analysis of Paraquat in Blood and Urine by Sodium Borohydride/Nickel Chloride Chemical Reduction-Gas Chromatography/Thermionic Specific Detector

HUANG LU-YAO1, LIAO LIN-CHUAN1, CHEN LI-LI1, SU GUI2, LI WEN-JIA2, HE RONG1, YAN YOU-YI1, YANG LIN1 (1. WEST CHINA SCHOOL OF PRECLINICAL AND FORENSIC MEDICINE, SICHUAN UNIVERSITY, CHENGDU 610041, CHINA; 2. WEST CHINA SCHOOL OF PHARMACY, SICHUAN UNIVERSITY   

  • Online:2008-12-25 Published:2008-12-28

被引次数

46

摘要： 目的建立血液和尿液中百草枯的还原反应-GC/TSD分析方法。方法生物样品经氯化钠盐酸溶液与氯仿-乙醇混合溶液去除蛋白后,上清液中目标物用硼氢化钠/氯化镍还原,乙酸乙酯提取,GC/TSD-热离子检测器分析,乙基百草枯为内标。结果血液和尿液中百草枯检测限(S/N=3)分别为0.002和0.004μg/mL;线性范围0.050～30.0μg/mL,相关系数r分别为0.999和0.998,方法回收率均大于80%。结论本方法准确、灵敏,重现性好,适用于体液中百草枯的检测。

关键词: 法医毒理学, 百草枯, 血液, 尿液, 硼氢化钠/氯化镍还原法, GC/TSD

Abstract: Objective To establish a new method for the analysis of paraquat in blood and urine by sodium borohydride/nickel chloride chemical reduction gas chromatography/ thermionic specific detector . Methods An initial procedure of precipitation was performed by adding hydrochloric solution with sodium chloride and a mixture of chloroform and ethanol. Then the analyte contained in supernatant was reduced by a reduction system of sodium borohydride and nickel chloride and extracted by acetic ether. Ethyl paraquat (EPQ) was used as internal standard. GC/TSD was used to identify and quantify the analyte. Results The limits of detection(S/N=3) in blood and urine were 0.002 and 0.004 μg/mL, respectively. The linear ranges were 0.050-30.0 μg/mL. Correlation coefficients in blood and urine were 0.999 and 0.998, respectively. The recoveries exceeded 80% both in blood and urine. Conclusion This method is applicable for quantification of paraquat in biological fluids.

Key words: forensic toxicology, paraquat, blood, urine, sodium borohydride/nickel chloride chemical reduction, GC/TSD