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建立了1个超高效液相色谱/静电场轨道阱高分辨质谱方法,对纸和纸制品中含氯酚进行了快速筛查和确证。19种含氯酚的色谱分离在Hypersil GOLD色谱柱(100mm×2.1mm,1.9μm)上进行,流动相为乙腈/氨水溶液(pH=10.5),采取梯度淋洗方式。质谱分析采用电喷雾负离子(ESI~-)模式,在m/z 50~m/z 300范围内进行一级质谱全扫描,利用保留时间和准分子离子的精确质量数进行快速筛查,19种含氯酚的质量数精确度误差均小于2×10~(-6)(2ppm);利用保留时间和二级质谱子离子进行确证。方法的定量限为0.5~2.0μg/kg,在3个不同加标浓度水平下,方法的平均加标回收率为81.96%~93.58%,相对标准偏差为3.25%~9.94%。采用该方法对市售纸制品进行快速筛查和确证,结果在1个样品中检出了五氯酚。
A super high performance liquid chromatography / electrostatic field orbitrap high resolution mass spectrometry method was established for the rapid screening and confirmation of chlorophenols in paper and paper products. The chromatographic separation of 19 chlorophenols was carried out on a Hypersil GOLD column (100 mm × 2.1 mm, 1.9 μm) using acetonitrile / ammonia solution (pH = 10.5) as the mobile phase and gradient elution. Mass spectrometry was carried out by first order mass spectrometry in the range of m / z 50 ~ m / z 300 with electrospray negative ion (ESI ~ -) mode. The first mass spectra were scanned completely by retention time and accurate mass of quasi- Chlorophenols were less than 2 × 10 -6 (2 ppm) in mass accuracy error, and confirmed by retention time and secondary ion mass spectrometry. The limit of quantification was 0.5-2.0 μg / kg. The average recoveries of the method were 81.96% -93.58% with relative standard deviations of 3.25% -9.94% at three spiked levels. Using this method, commercial paper products were rapidly screened and confirmed. As a result, pentachlorophenol was detected in one sample.