水蒸气蒸馏-气相色谱-质谱法测定皮革制品中19种含氯苯酚  

Determination of Nineteen Chlorophenols in Leather Products by Water Vapor Distillation-GC-MS

作　　者：胡苹 李大刚[1] 陈崇城[1] 王志文 HU Ping;LI Dagang;CHEN Chongcheng;WANG Zhiwen(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,泉州362000

出　　处：《理化检验（化学分册）》2020年第11期1205-1211,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：2019黎明职业大学科研团队项目(LMTD201901)。

摘　　要：为测定皮革制品中含氯苯酚的含量,在1.000g皮革样品中加入1mol·L^-1硫酸溶液20mL,用水蒸气蒸馏出样品中的含氯苯酚,馏出液和无水碳酸钾反应,含氯苯酚全部转化为含氯苯酚钾盐,经乙酸酐乙酰化后,所得衍生产物经DB-5MS毛细管色谱柱和程序升温分离,进入质谱仪,在电子轰击(EI)离子源和选择离子监测(SIM)模式下测定,内标法定量。结果表明:19种含氯苯酚质量浓度为1~40μg·L^-1时,其对应的乙酰化产物与内标物的乙酰化产物的质量浓度之比与相应的峰面积比呈良好的线性关系,检出限(3s)为0.006~0.015mg·kg^-1;以空白皮革制品为基质进行3个浓度水平的加标回收试验,回收率为85.7%~105%,相对标准偏差(n=6)为2.3%~8.0%。利用此方法分析了20个皮革制品,在5个样品中检出3,5-DiCP、2,4,6-TriCP、2,3,4,6-TeCP和PCP,检出值为0.20~1.11mg·kg^-1,共有5个检出值大于GB/T 18885-2009规定的限值(0.5mg·kg^-1)。To determine content of chlorophenols in leather products,1.000g of samples was taken and added into 20mL of 1mol·L^-1 sulfuric acid solution and the chlorophenols in sample were extracted by water vapor distillation.Distillate obtained was reacted with potassium carbonate,thus to have chlorophenols converted into chlorinated phenyl potassium salt.After acetylated by acetic anhydride,these accetates were separated by DB-5MS chromatographic column with programmed temperature,and then determined by MS under EI and SIM mode.An internal standard method was adopted for quantification.As shown by results,when the mass concentrition of 19 chlorophenols was in the range of 1-40μg·L^-1,ratio of mass concentration of their acetylation products between chlorophenols and the internal standard substance was linear with their respective ratios of peak area,with detection limits(3s)in the range of 0.006-0.015mg·kg^-1.The recovery was made on blank leather products by standard addition method at 3concentration levels,giving recoveries ranged from 85.7%to 105%.Values of RSDs(n=6)were found in the range of 2.3%-8.0%.The prescribed method was used for determination of 20leather products,3,5-DiCP,2,4,6-TriCP,2,3,4,6-TeCP and PCP were detected in 5samples,with detection values in the range of 0.20-1.11mg·kg^-1 and 5detected values over the limit value(0.5mg·kg^-1)given by GB/T 18885-2009.

关 键 词：水蒸气蒸馏 乙酰化衍生 气相色谱-质谱法 含氯苯酚 皮革制品 

分 类 号：O657.63[理学—分析化学]