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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
引用本文: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.
作者姓名:胡爱鹏  刘玉兰  张明明  陈 刚  安 骏
作者单位:1.河南工业大学粮油食品学院,河南 郑州 450001;2.中粮食品营销有限公司,北京 100020
基金项目:“十三五”国家重点研发计划专项(2016YFD0401400/2016YFD0401405)
摘    要:建立有机溶剂萃取、N-正丙基乙二胺(N-(n-propyl) ethylenediamine,PSA)玻璃固相萃取柱净化、内标法定量、气相色谱-质谱法直接测定植物油料中邻苯二甲酸二甲酯(dimethyl phthalate,DMP)、邻苯二甲酸二乙酯(diethyl phthalate,DEP)、邻苯二甲酸二异丁酯(di-iso-butyl phthalate,DIBP)、邻苯二甲酸二丁酯(dibutylphthalate,DBP)、邻苯二甲酸丁基苄基酯(butyl benzyl phthalate,BBP)、邻苯二甲酸二(2-乙基)己酯(di(2-ethtlhexyl) phthalate,DEHP)和邻苯二甲酸正辛酯(di-n-octyl phthalate,DNOP)7 种邻苯二甲酸酯的方法。该方法在0.01~2.0 mg/L范围内具有良好的线性关系,相关系数R2在0.999 8~1.000 0之间,仪器检出限(RSN=3)为0.01~0.02 μg/L,定量限(RSN=10)为0.03~0.06 μg/L。7 种目标物在0.1、0.5、1.0 mg/kg的加标水平下平均回收率为77.2%~98.8%,相对标准偏差为0.62%~9.37%(n=6)。采用本方法对不同种类、不同产地的76 个植物油料样品中7 种邻苯二甲酸酯类塑化剂含量进行测定。结果表明:所有受检植物油料样品中均检出DBP和DEHP,范围分别为(0.015±0.002)~(0.584±0.012) mg/kg和(0.085±0.006)~(2.334±0.016) mg/kg,检出率均为100%(76/76);DIBP、DEP、DMP、BBP、DNOP检出率分别为98.7%(75/76)、64.5%(49/76)、63.2%(48/76)、32.9%(25/76)、5.3%(4/76)。17 个油料样品中DBP含量超出国家标准限量(≤0.3 mg/kg),超标率为22.4%;1 个油料样品中DEHP含量超出国家标准限量(≤1.5 mg/kg),超标率为1.3%。

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  

Direct Determination of Phthalate Acid Esters in Oil Feedstock by Gas Chromatography-Mass Spectrometry
HU Aipeng,LIU Yulan,ZHANG Mingming,CHEN Gang,AN Jun.Direct Determination of Phthalate Acid Esters in Oil Feedstock by Gas Chromatography-Mass Spectrometry[J].Food Science,2016,37(18):146-151.
Authors:HU Aipeng  LIU Yulan  ZHANG Mingming  CHEN Gang  AN Jun
Affiliation:1. College of Food Science and Technology, Henan University of Technology, Zhengzhou 450001, China; 2. COFCO Food Sales & Distribution Co. Ltd., Beijing 100020, China
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 0.01–0.02 μg/L
and the limits of quantitation (LOQs) (RSN =10) ranged from 0.03 μg/L to 0.06 μg/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.
Keywords:oil feedstock  phthalate acid esters  solid-phase extraction  internal standard method  gas chromatography-mass spectrometry (GC-MS)  
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