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