固相萃取/高效液相色谱-串联质谱法测定罗非鱼中9种邻苯二甲酸酯

建立了罗非鱼中邻苯二甲酸二(2-甲氧基)乙酯(DMEP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二(2-丁氧基)乙酯(DBEP)、邻苯二甲酸二戊酯(DPP)、邻苯二甲酸二(4-甲基-2-戊基)酯(BMPP)、邻苯二甲酸二己酯(DHXP)、邻苯二甲酸二(2-乙基)己酯(DEHP)、邻苯二甲酸二正辛酯(DNOP)共9种邻苯二甲酸酯(PAEs)的高效液相色谱-串联质谱测定方法。样品经乙酸乙酯提取后,经LC-Si固相萃取柱净化,以甲醇和甲酸-乙酸铵缓冲溶液为流动相,梯度洗脱,采用HPLC-MS/MS电喷雾正离子(ESI+)电离,多反应监测(MRM)模式检测,基质匹配外标法定量。9种PAEs在1.0～200.0μg.L-1范围内均具有良好的线性关系,相关系数不低于0.991 8,平均加标回收率为75%～107%,批内、批间相对标准偏差分别在1.9%～11.8%和3.6%～13.1%之间。该方法具有简单、快速、灵敏度高和定性准确等优点,满足残留分析的要求。

Determination of Nine Phthalic Acid Esters in Tilapia by Solid Phase Extraction Coupled with High Performance Liquid Chromatography-Tandem Mass Spectrometry

A high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS)method was developed for the determination of nine PAEs,including bis(2-methoxyethyl) phthalate(DMEP),diethyl phthalate(DEP),benzyl butyl phthalate(BBP),bis(2-n-butoxyethyl) phthalate(DBEP),dipentyl phthalate(DPP),bis(4-methyl-2-pentyl) phthalate(BMPP),dihexyl phthalate(DHXP),bis(2-ethyl-h exyl) phthalate(DEHP)and di-n-octyl phthalate(DNOP) residues in tilapia sample.The samples were extracted with ethyl acetate,and purified with LC-Si solid-phase extraction column.Methanol and formic acid-ammonium acetate buffer were used as mobile phase by gradient elution.The analysis of target compounds was carried out by HPLC-MS/MS with positive electrospray ionization(ESI+) under multiple reaction monitoring(MRM) mode.A matrix matched external standard was used for the quantitative analysis.The calibration curves for nine PAEs were in good linearities between their peak areas and concentrations of 1.0-200.0 μg·L-1 with correlation coefficients not less than 0.991 8.The average spiked recoveries ranged from 75% to 107%.The relative standard deviations of intra-batch and inter-batch were in the ranges of 1.9%-11.8% and 3.6%-13.1%,respectively.The proposed method was simple,rapid,sensitive and accutate,and could meet the requirements for residue analysis.