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固相萃取-气相色谱法测定纺织品中的邻苯二甲酸酯类环境激素
引用本文:牛增元,叶曦雯,房丽萍,薛秋红,孙忠松.固相萃取-气相色谱法测定纺织品中的邻苯二甲酸酯类环境激素[J].色谱,2006,24(5):503-507.
作者姓名:牛增元  叶曦雯  房丽萍  薛秋红  孙忠松
作者单位:1.Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China; 2.College of Chemistry and Chemical Engineering, Ocean University of China, Qingdao 266003, China
基金项目:国家质量监督检验检疫总局科研项目
摘    要:采用索氏提取法以正己烷为提取溶剂提取纺织品中的邻苯二甲酸酯类物质(PAEs),以强阴离子交换固相萃取(SPE)小柱净化本底杂质并富集待测物,建立了纺织品中10余种PAEs环境激素的同时测定方法。采用的固相萃取条件为:5 mL正己烷活化、3 mL异辛烷淋洗、2 mL含15%乙酸乙酯的正己烷溶液洗脱。SPE能有效地对提取液进行富集浓缩,同时对纺织物提取液中的杂质净化效果突出。该方法准确可靠,重现性好,在5~100 mg/kg 添加水平,PAEs各化合物的回收率为86.3%~102.7%,相对标准偏差(RSD)一般小于5%。检测的10余种PAEs中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丙酯(DPrP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二戊酯(DAP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二环己酯(DCHP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)、邻苯二甲酸二正辛酯(DNOP)的方法检出限小于1mg/kg,邻苯二甲酸二异壬酯(DINP)与邻苯二甲酸二异癸酯(DIDP)的方法检出限分别为1.74 mg/kg和1.55 mg/kg。

关 键 词:固相萃取  气相色谱  邻苯二甲酸酯  环境激素  纺织品
文章编号:1000-8713(2006)05-0503-05
收稿时间:2005-10-20
修稿时间:2005年10月20

Determination of Phthalic Acid Esters in Textiles by Solid Phase Extraction-Gas Chromatography
NIU Zengyuan,YE Xiwen,FANG Liping,XUE Qiuhong,SUN Zhongsong.Determination of Phthalic Acid Esters in Textiles by Solid Phase Extraction-Gas Chromatography[J].Chinese Journal of Chromatography,2006,24(5):503-507.
Authors:NIU Zengyuan  YE Xiwen  FANG Liping  XUE Qiuhong  SUN Zhongsong
Institution:1.Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China; 2.College of Chemistry and Chemical Engineering, Ocean University of China, Qingdao 266003, China
Abstract:A method was established for the simultaneous determination of some phthalic acid esters,namely,dimethyl phthalate(DMP),diethyl phthalate(DEP),dipropyl phthalate(DPrP),dibutyl phthalate(DBP),diamyl phthalate(DAP),dihexyl phthalate(DHP),benzyl-n-butyl phthalate(BBP),di-(2-ethylhexyl)phthalate(DEHP),dicyclohexyl phthalate(DCHP),di-n-octyl phthalate(DNOP),diisononyl phthalate(DINP) and diisodecyl phthalate(DIDP) in textiles by solid phase extraction(SPE) coupled with gas chromatography(GC).The phthalic acid esters in textiles were extracted by Soxhlet extraction with hexane,the extracts were then cleaned up and enriched by a strong anion exchange(SAX) SPE cartridge.The parameters affecting the purification efficiency of SPE cartridge,such as solvent conditioning,rinsing,and elution,were studied.Conditioning with 5 mL hexane and rinsing with 3 mL isooctane were proved to be the optimal conditions.Of the several solvent ratios(ethylacetate in hexane) used for selective elution of phthalic acid esters from the SAX SPE cartridge,the 15%(v/v) content for ethylacetate in hexane gave the best result.Under the optimized conditions,the recoveries of phthalic acid esters for spiked standards(n=7) were 86.3%-102.7%,and the relative standard deviations(RSDs) were less than 5%.In this method the detection limits for DMP,DEP,DPrP,DBP, DAP,BBP,DCHP,DEHP,DNOP were all below 1 mg/kg,and the detection limits for DINP and DIDP were 1.74 mg/kg and 1.55 mg/kg respectively.This SPE-GC method is sensitive,accurate and suitable for the analysis of phthalate environmental hormones in textiles.
Keywords:solid phase extraction(SPE)  gas chromatography(GC)  phthalic acid esters  environmental hormones  textile
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