摘要
建立了以三氯化铁为催化剂,乙醇与尿中三氯乙烯的3种代谢产物(一氯乙酸、二氯乙酸、三氯乙酸)乙酯衍生化的气相色谱测定方法。对乙酯衍生化温度、时间、三氯化铁用量、乙醇用量进行探讨,确定了最优化的衍生条件为4 mL尿样加入1.05 mmol三氯化铁、2 mL乙醇,90℃水浴50 min,经2 mL正己烷萃取后直接进样测定。尿中一氯乙酸、二氯乙酸、三氯乙酸的浓度分别在40~2 400、20~1 000、10~500μg/L范围内呈良好线性,相关系数分别为0.999 8、0.999 3和0.999 2,3种氯代乙酸在尿样中的平均加标回收率为104%、109%和106%。方法的检出限分别为4.67、1.32、0.27μg/L。该方法乙酯衍生化试剂低毒、低腐蚀性,反应条件温和,操作简便,已成功用于三氯乙烯职业暴露人群尿样中3种代谢产物的生物检测。
A sensitive and reliable method was developed for the quantitative determination of three metabolites of trichloroethylene, e.g. monochloroacetic acid (MCA) , diehloroacetic acid (DCA) and trichloroacetic acid(TCA) , in urine sample. Three metabolites were derivatized by ethanol es- terification in the presence of ferric chloride acted. Effects of esterification temperature, esterification time and amounts of ferric chloride and ethanol were discussed, and the optimization conditions were using 4 mL urine sample mixed with 1.05 mmol ferric chloride and 2.0 mL ethanol to derivatize for 50 min in 90 ℃ water bath. The three ethyl esters in sample were simultaneously determined by derivatization gas chromatography coupled with electron-capture detection after extracted with 2 mL hexane. The method showed good linearities in the ranges of 40 - 2 400, 20 - 1 000 μg/L and 10 - 500 μg/ L for monochloroacetic acid, dichloroacetic acid and trichloroacetic acid, with correlation coefficients of 0. 999 8, 0. 999 3 and 0. 999 2, respectively. The average spiked recoveries of three metabolites in urine sample were 104% , 109% and 106% , with their detection limits(S/N =3) of 4.67, 1.32 and 0. 27 μg/L, respectively. With the advantages of simplicity, requirements for relatively moderate reaction condition and non-corrosion reagents, the method was applied in the quantitative analysis of three metabolites in the urine samples from workers exposed to the trichloroethylene contaminant with satisfactory results.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第3期377-380,共4页
Journal of Instrumental Analysis
基金
国家十一五科技支撑计划(2006BAI06B02)
广东省科技计划(2007B031512003)
广东省职业病防治重点实验室(2012A061400007)
关键词
一氯乙酸
二氯乙酸
三氯乙酸
衍生化
气相色谱
monochloroacetic acid
dichloroacetic acid
trichloroacetic acid
derivatization
gas chromatography