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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,2.6μm)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2.0~400μg/L范围内线性关系良好;方法定量限(S/N=10)在10μg/kg~30μg/kg之间;添加水平为10~300μg/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%。
A solid phase extraction (SPE) purification and ultra performance liquid chromatography tandem triple-quadrupole mass spectrometry (UPLC-MS / MS) was developed for the simultaneous determination of eight isothiazolinones and chlorophenols in food contact paper packaging materials (MI, CMI, BIT, 2,4-DCP, 2,4,6-TCP, 2,3,4,6-TCP, PCP and OPP). The sample was extracted by methanol and cleaned up by HLB solid phase extraction cartridge. The residue was separated on a Phenomenex kinetex C18 column (100 mm × 3.0 mm, 2.6 μm) using methanol-water as mobile phase. The electrospray positive and negative ions Segment scanning and multi-reaction monitoring (MRM) mode of detection, retention time and characterization ion pair qualitative, external standard quantitative. The results showed that there was a good linearity in the range of 2.0-400 μg / L for the 8 analytes; the limit of quantification (S / N = 10) was between 10 μg / kg and 30 μg / kg; , And the average recoveries ranged from 80.3% to 107%. The relative standard deviations (RSD, n = 6) ranged from 3.5% to 9.3%.