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

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

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。

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）, his （2-n-butoxyethyl） phthalate （ DBEP）, dipentyl phthalate （ DPP）, bis （4-methyl-2-pentyl） phthalate （BMPP） dihexyl phthalate （ DHXP）, his （ 2-ethyl-h exyl ） phthalate （DEHP） and di-n-octyl phthalate （ DN OP） residues in tilapia sample. The samples were extracted with ethyl acetate, and purified with LC - Si solid-phase extrac- tion column. Methanol and formic acid - ammonium acetate buffer were used as mobile phase by gra- dient elution. The analysis of target compounds was carried out by HPLC - MS/MS with positive elec- trospray ionization （ESI^＋） under multiple reaction monitoring （MRM） mode. A matrix matched exter- nal 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 coef- ficients not less than 0. 991 8. The average spiked recoveries ranged from 75% to 107% . The rela- tive 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.