高效液相色谱法测定人血液、尿液中的2,4-D丁酯

目的建立检测血液、尿液中2,4-D丁酯的高效液相色谱分析方法。方法采用正己烷为样品萃取溶剂,色谱柱为Zorbax SB-Aq柱,流动相为V（甲醇）∶V（水）=60∶40。结果 2,4-D丁酯在血液和尿液中的线性范围分别为0.10～10.00μg/mL（r≥0.999 8）和0.08～8.00μg/mL（r≥0.999 5）,检测限分别为0.002 0μg/mL和0.001 8μg/mL,准确度为94.5%～104.5%,日内、日间精密度≤4.5%。结论本研究建立的血液、尿液中2,4-D丁酯的提取和HPLC检测方法,可应用于2,4-D丁酯中毒的快速检验和中毒死亡的法医学鉴定。

Determination of 2,4-D Butyl Ester in Blood and Urine by HPLC

Objective To establish a HPLC method for determination of 2,4-D butyl ester in blood and urine.Methods Compound was extracted from blood and urine using ethyl acetate.Separation was achieved on Zorbax SB-Aq column using methanol-water（60：40） as mobile phase.Results The calibration curve of 2,4-D butyl ester ranged from 0.10 μg/mL to 10.00 μg/mL in blood（r≥0.999 8） and 0.08 μg/mL to 8.00 μg/mL in urine（r≥0.999 5）,respectively.The limits of detection for the analyte was 0.002 0 μg/mL and 0.001 8 μg/mL in blood and urine,respectively.The intra and inter day assay precision were no more than 4.5%.The mean recovery ranged from 94.5% to 104.5%.Conclusions The pre-treatment and HPLC analysis of 2,4-D butyl ester in blood and urine can be used for rapid diagnosis of 2,4-D butyl ester poisoning and forensic identification of 2,4-D butyl ester poisoning death.