[1]严煌倩,李勇,翟丽菲,等.气相色谱-质谱法结合QuEChERS法快速检测青椒中15种邻苯二甲酸酯[J].江苏农业学报,2018,(02):459-465.[doi:doi:10.3969/j.issn.1000-4440.2018.02.034]
　YAN Huang-qian,LI Yong,ZHAI Li-fei,et al.Determination of 15 phthalate acid esters in pepper by gas chromatography-mass spectrometry with QuEChERS method[J].,2018,(02):459-465.[doi:doi:10.3969/j.issn.1000-4440.2018.02.034]
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气相色谱-质谱法结合QuEChERS法快速检测青椒中15种邻苯二甲酸酯()
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江苏农业学报[ISSN:1006-6977/CN:61-1281/TN]

卷:
期数:
2018年02期
页码:
459-465
栏目:
加工贮藏·质量安全
出版日期:
2018-04-25

文章信息/Info

Title:
Determination of 15 phthalate acid esters in pepper by gas chromatography-mass spectrometry with QuEChERS method
作者:
严煌倩1; 2; 3; 李勇2; 3; 翟丽菲2; 3; 龙玲2; 3; 程金金2; 3; 陈小龙2; 3; 葛静2; 3; 杨丽璇2; 3; 余向阳2; 3
（1.南京财经大学食品科学与工程学院，江苏省现代粮食流通与安全协同创新中心，江苏高校粮油质量安全控制及深加工重点实验室，江苏南京210023；2.江苏省农业科学院农产品质量安全与营养研究所，江苏南京210014；3.省部共建国家重点实验室培育基地-江苏省食品质量安全重点实验室，江苏南京210014）
Author(s):
YAN Huang-qian1; 2; 3; LI Yong2; 3; ZHAI Li-fei2; 3; LONG Ling2; 3; CHENG Jin-jin2; 3; CHEN Xiao-long2; 3; GE Jing2; 3; YANG Li-xuan2; 3; YU Xiang-yang2; 3
（1.College of Food Science and Engineering/Collaborative Innovation Center for Modern Grain Circulation and Safety/Key Laboratory of Grains and Oils Quality Control and Processing, Nanjing University of Finance and Economics, Nanjing 210023, China；2.Institute of Food Safety and Nutrition， Jiangsu Academy of Agricultural Sciences, Nanjing 210014, China;3.Key Lab of Food Quality and Safety of Jiangsu Province-State Key Laboratory Breeding Base, Nanjing 210014, China)
关键词:
邻苯二甲酸酯; QuEChERS法; 气相色谱-质谱法; 青椒
Keywords:
phthalate acid esters; QuEChERS method; gas chromatography-mass spectrometry; pepper
分类号:
O658;TS207.3
DOI:
doi:10.3969/j.issn.1000-4440.2018.02.034
文献标志码:
A
摘要:
为了建立同时检测青椒中15种邻苯二甲酸酯类化合物（PAEs）的方法，将QuEChERS法与气相色谱-质谱法相结合，样品用乙腈超声振荡提取，经乙二胺-N-丙基合硅胶（PSA）、石墨化碳（GCB）吸附剂净化，用DB-5MS色谱柱程序升温分离，在选择离子监测模式（SIM）下进行测定。15种邻苯二甲酸酯的质量浓度在10.0 μg/kg 至1 000.0 μg/kg范围内与峰面积的线性关系较好（r≥0.997 5），检出限（S/N=3）为0.1～0.7 μg/kg，定量限（S/N=10）为 0.3～2.1 μg/kg，加标回收率为 70.3%～108.0%，相对偏差（RSD）值为 1.4%～10.2%。结果表明，该方法快速、灵敏，符合多残留检测和痕量分析的技术要求，适用于蔬菜中邻苯二甲酸酯类残留的分析。测定大棚青椒样品，邻苯二甲酸酯含量为 248.45～343.96 μg/kg，其中邻苯二甲酸二丁酯（DBP）、邻苯二甲酸二（2-乙基）己酯（DEHP）和邻苯二甲酸二异丁酯（DIBP）残留量较高。
Abstract:
Gas chromatography-mass spectrometry (GC-MS) coupled with QuEChERS method was established for the simultaneous detection of 15 phthalate acid esters (PAEs) residues in pepper. The pepper samples were extracted by ultrasound and shaker with acetonitrile, then purified by ethylenediamine-N-propyl silane (PSA) and graphitized carbon black (GCB) adsorbent. The 15 phthalate esters were separated on a DB-5MS column with temperature programming, and detected quantitatively under the selective ion monitoring mode (SIM). Under the optimization method, a good linearity was obtained in the range of 10.0-1 000.0 μg/kg, and the correlation coefficients were large than 0.997 5. The detection limits (S/N=3) for 15 PAEs were 0.1-0.7 μg/kg, and the limits of quantitation were 0.3-2.1 μg/kg. The average recoveries of the method ranged from 70.3% to 108.0%, and the relative standard deviations (RSD) were 1.4%-10.2%. The results showed that this method was accurate and sensitive to meet the requirements of multiple residues determination, and could be applied in the analysis of phthalate esters residues in vegetables. The content of phthalates ranged from 248.45 μg/kg to 343.96 μg/kg, and the contents of dibutyl phthalate (DBP), di(2-ethyl)hexyl phthalate (DEHP) and diisobutyl phthalate (DIBP) were higher.

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备注/Memo

备注/Memo:
收稿日期：2017-08-20 基金项目：国家自然科学基金项目（31371798、31601665）；江苏省自然科学基金项目（BK20160576）；国家农产品质量安全风险评估基金项目（GJFP201701102）；江苏省农业科学院基金项目（6111672） 作者简介：严煌倩（1992-），女，江苏南通人，硕士研究生，主要从事农产品安全研究工作。（E-mail）1191096770@qq.com 通讯作者：余向阳，(E-mail）yu981190@hotmail.com
更新日期/Last Update: 2018-05-04