摘要
采用乙醇对氯乙酰氯及其多氯杂质(二氯乙酰氯、三氯乙酰氯)进行柱前衍生化,通过高效液相色谱法测定氯乙酰氯及其多氯杂质的含量。在选定的色谱条件下,即采用Hedera ODS-2液相色谱柱,以乙腈/水(60/40)为流动相(每500 mL流动相中含0.68 g磷酸二氢钾),检测波长为210 nm,氯乙酰氯及其多氯杂质衍生物能得到有效分离,并能获得较好的检测效果。氯乙酰氯、二氯乙酰氯、三氯乙酰氯的线性相关系数分别为0.9999、0.9995、0.9998,回收率分别为98.66%~99.63%、98.24%~101.63%、97.84%~102.45%,变异系数分别为0.42%、2.92%、3.27%,最低检出限分别为0.14 mg/L、0.24 mg/L、0.21 mg/L。
Chloroacetyl chloride and its multichloroacetyl chloride impurities(dichloroacetyl chloride,trichloroacetyl chloride) were pre-column derivatized with ethanol,and the content of chloroacetyl chloride and its multichloroacetyl impurities was determined by high performance liquid chromatography.Under the selected chromatographic conditions,that is,using Hedera ODS-2 LC column,with acetonitrile/water(60/40)as mobile phase(0.68 g potassium dihydrogen phosphate per 500 mL mobile phase),the detection wavelength is 210 nm,chloroacetyl chloride and its multichloroacetyl chloride impurity derivatives can be effectively separated,and a better detection effect can be obtained.The linear correlation coefficients of chloroacetyl chloride,dichloroacetyl chloride and trichloroacetyl chloride were 0.9999,0.9995 and 0.9998,respectively.The recoveries were 98.66%~99.63%,98.24%~101.63%,and 97.84%~102.45%,respectively.The coefficients of variation were 0.42%,2.92%,and 3.27%,respectively.And the minimum detection limits were 0.14 mg/L,0.24 mg/L,and 0.21 mg/L,respectively.
作者
段文胜
刘益红
DUAN Wen-sheng;LIU Yi-hong(Oriental(Luzhou)Agrochemicals Co.,Ltd.,Luzhou,Sichuan 646300,China)
出处
《浙江化工》
CAS
2022年第2期47-49,54,共4页
Zhejiang Chemical Industry
关键词
氯乙酰氯
多氯乙酰氯
高效液相色谱
柱前衍生化
chloroacetyl chloride
multichloroacetyl chloride
high performance liquid chromatography(HPLC)
per-column
