分析测试学报2013，Vol.32Issue(8)：915-922,8.DOI:10.3969/j.issn.1004-4957.2013.08.002
气相色谱-质谱法测定水产品中15种邻苯二甲酸酯类塑化剂的残留量
Determination of Fifteen Types of Phthalic Acid Esters.Plasticizer Residues in Aquatic Products by Gas Chromatography-Mass Spectrometry
摘要
Abstract
A method was developed for the simultaneous determination of 15 phthalic acid esters at trace level in aquatic products by solid phase extraction(SPE) purification coupled with gas chromatography-mass spectrometry(GC-MS).The PAEs were extracted with dichloromethane-hexane (1 ∶ 1) by ultrasonic-assisted technique,then purified with SPE glass column packed with 3.0 g neutral alumina caped with approximately 2 cm anhydrous sodium sulfate on the top.The target analyres were eluted with hexane,dichloromethane-hexane (1 ∶ 9) mixture,ethyl acetate-hexane (1 ∶ 4)mixture,and ethyl acetate,sequentially.The eluent was evaporated to near dryness,and redissolved in 1 mL hexane,and analyzed by GC-MS under the selected ion monitoring mode.Under optimized conditions,the linear ranges of 15 phthalic acid esters were in the range of 0.05-1.0mg/L with correlation coefficients(r) not less than 0.999 1.The average recoveries of 15 phthalic acid esters in different kinds of fishery products samples at spiked levels of 2,50,200 μg/kg were in the range of 81％-123％,with relative standard deviations(RSDs,n =3) less than 15％.The limits of detection(LOD,S/N =3) ranged from 0.04 μg/kg to 1.18 μg/kg,and the limits of quantitation(LOQ,S/N =10) ranged from 0.20 μg/kg to 4.00 μg/kg.The proposed method is suitable for the simultaneous determination of 15 phthalic acid esters in fishery products with easy operation,high accuracy and precision.关键词
邻苯二甲酸酯/水产品/气相色谱-质谱Key words
phthalic acid esters (PAEs) / aquatic products/ gas chromatography-mass spectrometry(GC-MS)分类
化学化工引用本文复制引用
石凤琼,柯常亮,林钦,孙闰霞..气相色谱-质谱法测定水产品中15种邻苯二甲酸酯类塑化剂的残留量[J].分析测试学报,2013,32(8):915-922,8.基金项目
中央级公益性科研院所基本科研业务费专项(2012TS15) （2012TS15）
农业部水产品加工重点实验室开放基金(nybjg201204) （nybjg201204）
