UPLC-MS/MS法同时测定食品接触纸包装材料中的异噻唑啉酮类和氯酚类杀菌防腐剂

Simultaneously Detecting Chlorophenols and Isothiazolinones in Food Contact Paper Packaging Materials using Ultrahigh-performance Liquid Chromatography Tandem Mass Spectrometry

摘要:

建立了固相萃取（SPE）净化，超高效液相色谱串联三重四极杆质谱法（UPLC- MS/MS）同时检测食品接触纸包装材料中8种异噻唑啉酮类和氯酚类杀菌防腐剂（MI、CMI、BIT、2,4-DCP、2,4,6-TCP、2,3,4,6-TCP、PCP和OPP）的分析方法。样品经甲醇超声提取，HLB固相萃取小柱净化，以甲醇-水为流动相在Phenomenex kinetex C18色谱柱（100 mm×3.0 mm，2.6 μm）上梯度洗脱分离，在电喷雾正、负离子分段扫描和多反应监测（MRM）模式下检测，以保留时间和特征离子对定性，外标法定量。结果表明，8种待测物在2.0~400 μg/L范围内线性关系良好；方法定量限（S/N=10）在10 μg/kg~30 μg/kg之间；添加水平为10~300 μg/kg时，平均回收率在80.3%~107%之间；相对标准偏差（RSD，n=6）为3.5%~9.3%。

Abstract:

A comprehensive analytical method was developed to simultaneously detect chlorophenols and isothiazolinones (MI, CMI, BIT, 2,4-DCP, 2,4,6-TCP, 2,3,4,6-TCP, PCP, and OPP) in food contact paper packaging materials using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and solid phase extraction (SPE). The paper samples were subjected to ultrasonic methanol extraction, concentrated, and purified with an Oasis HLB SPE cartridge. The extract was separated in a Phenomenex Kinetex C18 column (100 mm × 3.0 mm, 2.6 μm) using gradient elution with a methanol-water mobile phase. The MS/MS analysis was performed in electrospray ionization mode with multiple reaction monitoring (MRM) and separated into two segments of positive and negative ionization modes. Eight compounds were identified by retention time and the ratio of characteristic ions, and these were quantified using the external standard methods. Under optimal conditions, the calibration curves for the eight analytes were linear within the range of 2.0 to 400 μg/L, with correlation coefficients more than 0.997. The quantitation limits of the method (S/N=10) for the eight compounds were 10 to 30 μg/kg. The mean recoveries for paper samples at spiked concentration levels of 10 to 300 μg/kg were between 80.3% and 107%, while the relative standard deviations (RSDs, n = 6) ranged from 3.5% to 9.3%.