ID-MSPD-UHPLC-MS/MS检测烘焙食品及原料中的8种酚类污染物

Determination of 8 Phenols in Bakery Food and Raw Material by Isotope Dilution - Dispersive Solid Phase Extraction Couple with UHPLC-MS/MS

摘要:

建立了同位素稀释（isotope dilution，ID），基质分散固相萃取（dispersive solid phase extraction，DSPE）结合液相色谱串联质谱（UHPLC-MS/MS）检测烘焙食品及原料（面粉、面粉改良剂、蛋黄馅等）中双酚类污染物（双酚A、双酚B、双酚C、双酚F、双酚S、双酚AF）、紫外吸收剂UV-0和抗氧化剂TH1790的方法。样品经乙腈提取，C18分散吸附剂净化（蛋黄馅料等油脂含量高的样品先用正己烷出去油脂）后，采用C18色谱柱、乙腈-氨水为流动相梯度洗脱分离，以负离子（ESI-）多方应监测模式（schedule MRM）进行检测，内标法定量。8种酚类污染物在1.0~200.0 μg/L范围内线性良好，相关系数(R2)在0.999以上。仪器检出限（LODs）0.5~5.0 μg/L，加标回收率82.10%~113.20%，相对标准偏差为2.70%~9.50%。方法前处理简单，选择性强，灵敏度高，可满足烘焙食品及其原料中8种酚类污染物的检测。

Abstract:

A method based on isotope dilution (ID), dispersive solid phase extraction (DSPE) couple with UHPLC-MS/MS was presented for determination of 8 phenols, including 4,4’-Isopropylidenediphenol (BPA), 4, 4'-(1-methylpropylidene) bisphenol (BPB), 4,4'- (2,2-Dichlorovinylidene) bisphenol (BPC), 4, 4'-methylene diphenol (BPF), 4, 4'-Sulfonyldiphenol (BPS), 4,4'- (Hexafluoroisopropylidene) diphenol (BPAF), 2,4-Dihydroxybenzophenone (UV-0) and 2,4-Dihydroxybenzophenone (TH1790) in bakery food and raw material (Flour, Flour-improving Agent, Egg Yolk filling et al.). Target compound was extracted by acetonitrile, and purified by C18 dispersion adsorbent (for high oil content such as egg yolk filling, extra fats were removed beforehand by hexane). A total of 8 targets were separated on a C18 column by gradient elution with acetonitrile-ammonium hydroxide as mobile phase, ionized with negative electrospray ionization (ESI -), detected under the schedule of multiple reaction monitoring (schedule-MRM) mode, and quantified with internal standard method. A favorable linearity was acquired in the concentration range of 1.0~200.0 μg/L with the correlation coefficients (R2) better than 0.999, and the limits of detection (LODs) were ranged from 0.5 to 5.0 μg/L. The spiked average recoveries presented 82.10%~113.20%, with the relative standard deviation (RSD, n = 6) of 2.70%~9.50%. These methods are rapid, sensitive and suitable for the determination of 8 Phenols in bakery food and raw material.