食品科学2016，Vol.37Issue(18)：146-151,6.DOI:10.7506/spkx1002-6630-201618024
气相色谱-质谱联用法直接测定植物油料中邻苯二甲酸酯类塑化剂
Direct Determination of Phthalate Acid Esters in Oil Feedstock by Gas Chromatography-Mass Spectrometry
摘要
Abstract
A method for the analysis of seven phthalate acid esters (PAEs) including dimethyl phthalate (DMP), diethyl phthalate (DEP), di-iso-butyl phthalate (DIBP), dibutyl phthalate (DBP), di (2-ethtlhexyl) phthalate (DEHP), butyl benzyl phthalate (BBP) and di-n-octyl phthalate (DNOP) in oil feedstock by gas chromatography-mass spectrometry (GC-MS) was established. In this method, sample pretreatment was achieved by organic solvent extraction and subsequent purification by N-(n-propyl) ethylenediamine (PSA) solid-phase extraction (SPE), and the analytes were analyzed by GC-MS with internal standard calibration. The proposed calibration curves had good linearity in the range of 0.01–2.0 mg/L with correlation coefficients between 0.999 8 and 1.000 0. The limits of detection (LODs) (RSN =3) of this method were 0.01–0.02μg/L and the limits of quantitation (LOQs) (RSN=10) ranged from 0.03μg/L to 0.06μg/L. The average recoveries of 7 PAEs varied from 77.2% to 98.8% with relative standard deviation (LSDs) of 0.62%–9.37% (n= 6) at the spiked levels 0.1, 0.5, and 1.0 mg/kg. The contents of 7 PAEs (DMP, DEP, DBP, DIBP, BBP, DEHP, and DNOP) in 76 oil feedstock samples from different species and geographic origins were determined by this method. The results showed that DBP and DEHP were detected in all these samples, ranging from (0.015± 0.002) to (0.584± 0.012) mg/kg and from (0.085± 0.006) to (2.334± 0.016) mg/kg, respectively. The detection rates of DIBP, DEP, DMP, BBP, and DNOP were 98.7% (75/76), 64.5% (49/76), 63.2% (48/76), 32.9% (25/76), and 5.3% (4/76), respectively. Of the 76 samples, the contents of DBP in 17 samples (22.4%) and DEHP in 1 sample (1.3%) exceeded the maximum limit stipulated in the national standard as 0.3 mg/kg for DBP and 1.5 mg/kg for DEHP.关键词
植物油料/邻苯二甲酸酯/固相萃取/内标法定量/气相色谱-质谱法Key words
oil feedstock/phthalate acid esters/solid-phase extraction/internal standard method/gas chromatography-mass spectrometry (GC-MS)分类
轻工纺织引用本文复制引用
胡爱鹏,刘玉兰,张明明,陈刚,安骏..气相色谱-质谱联用法直接测定植物油料中邻苯二甲酸酯类塑化剂[J].食品科学,2016,37(18):146-151,6.基金项目
“十三五”国家重点研发计划专项 （）
