气相色谱-电子捕获负化学源质谱法测定皮革中10种含氯苯酚  

Determination of ten chlorophenols in leather by gas chromatography-mass spectrometry with electron capture negative ionization

作　　者：胡苹 李大刚[1] 陈晓玲[1] 王开明 HU Ping;LI Da-gang;CHEN Xiao-ling;WANG Kai-ming(Department of Materials and Chemical Engineering,Liming Vocational University,Quanzhou 362000,China)

机构地区：[1]黎明职业大学材料与化学工程学院,福建泉州362000

出　　处：《化学研究与应用》2020年第10期1905-1910,共6页Chemical Research and Application

基　　金：2019黎明职业大学科研团队项目(LMTD201901)资助。

摘　　要：建立了气相色谱-电子捕获负化学源质谱法同时测定皮革中10种含氯苯酚的分析方法。样品中10种含氯苯酚化合物经水蒸气蒸馏萃取,萃取液经乙酸酐乙酰化后以正己烷萃取,经DB-5MS毛细管气相色谱柱分离,质谱采用电子捕获负化学源模式,反应气采用甲烷。结果表明:10种含氯苯酚化合物含量在1~40μg·L^-1范围内呈良好的线性关系,线性相关系数(r^2)>0.995,方法检出限为0.005~0.016 mg·kg^-1,在3个加标水平下的平均回收率为87.5%~117.4%,相对标准偏差(RSD,n=6)为1.1%~8.7%。方法能够满足对皮革中10种含氯苯酚化合物的分析要求。A method was developed for the determination of 10 chlorophenols in leather by gas chromatography-mass spectrometry with electron capture negative ionization.10 chlorophenols in samples were extracted by steam distillation.The extract was acetylated by acetic anhydride with n-hexane extraction after acetylation.The extract was separated by DB-5MS glass capillary column,and quantification was performed by mass spectrometry with electron capture negative ionization using methane as chemical ionization reagent.The calibration curves of 10 CPs were linear in the range of 1~40μg·L^-1 with correlation coefficients(r^2)more than 0.995.The detection limits of compounds were 0.005~0.016 mg·kg^-1.The spiked average recoveries varied from 87.5%^-117.4%at three spiked levels with relative standard deviation(RSD,n=6)of 1.1%-8.7%.The proposed method was rapid,simple,sensitive and accurate,which was suitable for the determination of ten chlorophenols in leather products.

关 键 词：电子捕获负化学源 气相色谱 皮革 含氯苯酚 

分 类 号：O657.7[理学—分析化学]