色谱2016，Vol.34Issue(5)：502-511,10.DOI:10.3724/SP.J.1123.2015.12035
气相色谱-三重四极杆串联质谱法同时测定焙烤食品中28种邻苯二甲酸酯
Determination of 28 phthalate esters in baked foods by gas chromatography-triple quadrupole mass spectrometry
摘要
Abstract
An efficient method using gas chromatography-triple quadrupole mass spectrometry for the determination of 28 phthalate ester residues in bakery foods was established. The samples were extracted with ethyl acetate,and cleaned up with neutral alumina. The separation was per-formed on a TR-5MS capillary column( 30 m × 0. 25 mm × 0. 25 μm )by programmed temperature vaporization( PTV)with splitless mode. Meanwhile the identification and quantification were per-formed by GC-MS/MS in selected reaction monitoring(SRM)mode and using the internal stand-ard method. The calibration curves of the 27 phthalate esters showed good linearities in the range of 0. 05-10 mg/L,except diisononyl ortho-phthalate( DINP)which was in the range of 0. 1-20 mg/L,with the correlation coefficients not less 0. 996 2. The limits of detection( LODs)were 0. 1-9. 8 μg/kg and the limits of quantification( LOQs)were 0. 4-32. 6 μg/kg. With the proposed method,the spiked recoveries were evaluated in four types of baked foods( bread,biscuits, cakes,stuffing)at low,medium and high concentrations. The results showed that the average recoveries of the 28 PAEs were in the range of 81. 0%-117%,and the relative standard deviations (RSDs,n=6)were in the range of 1. 3%-13. 6%. The method was successfully applied in the investigation of the PAEs distribution in baked foods. The method is suitable for the determina-tion of the 28 PAEs in baked foods with easy operation,high accuracy and precision.关键词
气相色谱-三重四极杆串联质谱/邻苯二甲酸酯/塑化剂/焙烤食品Key words
gas chromatography-tandem mass spectrometry( GC-MS/MS )/phthalate eaters ( PAEs)/plasticizer/baked foods分类
化学化工引用本文复制引用
李蓉,薄艳娜,卢俊文,林勤保,黄志强,陈丽斯..气相色谱-三重四极杆串联质谱法同时测定焙烤食品中28种邻苯二甲酸酯[J].色谱,2016,34(5):502-511,10.基金项目
国家科技支撑计划课题（2012BAK08B01）；广东省省级科技计划项目（2014A040401011）；国家质检总局科技计划项目（2015IK260）；中山市社会公益重大专项（2015B2295）．@@@@National Key Technology R．&D． Program（ No．2012BAK08B01）；Science and Technology Planning Project of Guangdong Province of China（ No．2014A040401011）；Science and Technology Planning Project of Gen-eral Administration of Quality Supervision，Inspection and Quarantine of the People’s Republic of China （ AQSIQ）（ No．2015IK260）；Social Public Welfare Major Project of Zhongshan City（ No．2015B2295）． （）
