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固相萃取-气相色谱-质谱法分析火腿肠中邻苯二甲酸酯的方法开发与应用。

Development and application of a method for analysis of phthalates in ham sausages by solid-phase extraction and gas chromatography-mass spectrometry.

机构信息

Faculty of Materials Science and Chemical Engineering, The State Key Laboratory Base of Novel Functional Materials and Preparation Science, Ningbo University, Ningbo, Zhejiang 315211, PR China.

出版信息

Meat Sci. 2010 Mar;84(3):484-90. doi: 10.1016/j.meatsci.2009.10.002. Epub 2009 Oct 8.

Abstract

A gas chromatography-mass spectrometry assay was developed and successfully applied for the determination of phthalates in ham sausage migrated from packaging film. The phthalates studied were dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), benzylbutyl phthalate (BBP), bis(2-ethylhexyl) phthalate (DEHP) and di-n-octyl phthalate (DNOP), with dibutyl adipate (DBA) as internal standard. The sample pre-treatments included extraction with n-hexane, solvent evaporation and reconstitution with acetonitrile before and after solid-phase extraction (SPE). The extraction and cleaning up procedure was carried out with cartridges containing dimethyl butylamine groups, which showed extraction efficiencies over 87.3%. The calibration curves obtained were linear with correlation coefficients greater than 0.99. The method proved to be accurate and precise for the six phthalates used. It was successfully applied to a study on the migration of phthalates from packaging PVC film into ham sausage.

摘要

建立了一种气相色谱-质谱联用测定方法,成功地应用于从包装薄膜中迁移到火腿肠中的邻苯二甲酸酯的测定。研究的邻苯二甲酸酯包括邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)和邻苯二甲酸二正辛酯(DNOP),以邻苯二甲酸二丁酯(DBA)为内标。样品预处理包括用正己烷提取、溶剂蒸发以及在固相萃取前后用乙腈重新溶解。萃取和净化过程采用含有二甲基丁基胺基团的小柱进行,萃取效率超过 87.3%。得到的校准曲线具有大于 0.99 的相关系数,呈线性关系。该方法对六种邻苯二甲酸酯的测定结果准确、精密。该方法成功地应用于研究包装 PVC 薄膜向火腿肠中迁移邻苯二甲酸酯的情况。

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