尿中3种苯氧羧酸类除草剂的气相色谱分析法

The Gas Chromatographic Analytical Methods for the Determination of Three Phenoxy Acid Herbicides in Urine

本文研究了2,4-滴、2,4-滴丙酸和2甲4氯3种苯氧羧酸类除草剂用硫酸、三氯化硼、氯化氢和三氟乙酸等4种催化剂的甲醇、乙醇、丙醇、丁醇、戊醇、苯甲醇、三氟乙醇、五氟丙醇、二氯丙醇和五氟苯甲醇等10种醇的酯化衍生反应条件,在此基础上建立了尿中3种苯氧羧酸类除草剂的各种衍生化气相色谱电子俘获检测方法,其中较灵敏的方法2,4-滴和2,4-滴丙酸的检出限低于10 ng/mL,2甲4氯的检出限低于20ng/mL,适于职业接触者和中毒者的尿分析。

In this paper the reaction conditions of esterifying derivatization of 2,4-D, 2,4-DP, and MCPA with methanol, ethanol, n-propanol, n-butanol, n-pentanol, benzylalcohol, trifluoroethanol, pentaflouropropanol, 1,3-dichloropropan-2-ol, and pentafluorobenzyl alcohol using sulfuric acid, boron trichloride, hydrogen chloride and trifluoroacetic acid as catalyst were studied. The hydrogen chloride and trifluoroacetic acid was respectively produced by reaction of acetyl chloride or trifluoroacetic acid aldehyde with trace water in reaction system. At the base of this investigation, the analytical methods of the three herbicides in urine using various esterifying derivatizition and gas chromatography with electron capture detection were developed. The detection limits of the most sensitive method for 2,4-D and 2,4-DP were below 10 ng/mL, and that for MCPA was below 20 ng/mL. The linear relationships and recoveries of some sensitive methods were determined. The results were satisfactory. The sensitive methods developed in this paper are suitable for urinary analysis of poisoning subjects and occupationally exposed subjects.