摘要
建立气相色谱-三重四极杆串联质谱同时测定食用油中的18种邻苯二甲酸酯、16种多环芳烃和7种多氯联苯的检测方法。样品经正己烷饱和乙腈超声提取、固相萃取柱净化,采用DB-5毛细管柱分离,以电子电离源,多反应离子监测模式定量测定。该方法邻苯二甲酸酯类塑化剂的线性范围为0.04~2 mg/kg,其中邻苯二甲酸二异壬酯的线性范围为1~40 mg/kg,多环芳烃和多氯联苯的线性范围为0.01~0.4 mg/kg,各物质在相应质量浓度范围内线性关系良好,相关系数均大于0.99。方法检出限范围为0.08~2μg/kg(除邻苯二甲酸二异壬酯的检出限为8μg/kg),回收率在62.7%~128.3%之间,相对标准偏差在1.1%~13.6%之间(n=6)。该方法准确、灵敏、简单、快速,可用于食用油中18种邻苯二甲酸酯、16种多环芳烃和7种多氯联苯的定量测定。
In this paper,a gas chromatography-tandem mass spectrometry(GC-MS)method was established for the determination of 18 phthalates,16 polycyclic aromatic hydrocarbons and 7 polychlorinated biphenyls in edible oils.The sample was ultrasonically extracted with acetonitrile saturated by n-hexane,and the extract was cleaned up by solid phase extraction(SPE),separated on a DB-5 capillary column,ionized by electron impact and quantitated in the selective reaction monitor(SRM)mode.Good linearity was observed for all the analytes in the concentration ranges tested(0.04–2 mg/kg for phthalate acid esters,1–40 mg/kg for diisodecyl phthalate(DINP),and 0.01–0.4 mg/kg for polycyclic aromatic hydrocarbons and polychlorinated biphenyls),with correlation coefficients more than 0.99.The limits of detection(LODs)were 8μg/kg for DINP and 0.08–2μg/kg for the other compounds.The recoveries ranged from 62.7%to 128.3%,with relative standard deviations(RSDs)of 1.1%to 13.6%(n=6).The method was sensitive,accurate,simple,rapid and thus suitable for the detection of phthalate acid esters,polycyclic aromatic hydrocarbons and polychlorinated biphenyls in edible oils.
作者
孟维一
古瑾
姜锐
张晴
赵文涛
马燕红
赵奕昕
李莹莹
郭文萍
MENG Weiyi;GU Jin;JIANG Rui;ZHANG Qing;ZHAO Wentao;MA Yanhong;ZHAO Yixin;LI Yingying;GUO Wenping(China Meat Research Center,Beijing 100068,China;College of Life Science and Bio-engineering,Beijing University of Technology,Beijing 100020,China)
出处
《食品科学》
EI
CAS
CSCD
北大核心
2020年第4期300-306,共7页
Food Science
基金
北京市优秀人才培养资助项目(2016754154700G147)
国家重点研发计划“食品安全关键技术研发”重点专项(2017YFC1601706)
关键词
气相色谱-三重四极杆串联质谱
邻苯二甲酸酯
多环芳烃
多氯联苯
食用油
gas chromatography-tandem mass spectrometry
phthalates
polycyclic aromatic hydrocarbons
polychlorinated biphenyls
edible oils