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以甲醇为溶剂,85℃下微波萃取皮革及其制品中的乙二醇醚类有机溶剂,萃取物经固相萃取柱净化后进行气相色谱-质谱/选择离子监测法测定,外标法定量,从而建立了同时测定皮革及其制品中12种乙二醇醚类有机溶剂残留量的气相色谱-质谱联用方法。该方法的加标回收率为81.1%~95.9%,相对标准偏差(RSD,n=9)为1.4%~9.6%。在信噪比(S/N)为10的条件下,各组分的定量下限(LOQ)为0.05~0.20mg/kg。该方法操作简单、方便快速、灵敏度高,可满足皮革及其制品中乙二醇醚类有机溶剂残留量检测的技术要求,并为制定相关检测标准提供了参考。
Using methanol as solvent, 85 ℃ microwave extraction of leather and its products of glycol ether organic solvents, extracts by solid phase extraction column after gas chromatography - mass spectrometry / selected ion monitoring method, external standard method, A gas chromatography-mass spectrometry (GC-MS) method was established for the simultaneous determination of 12 kinds of glycol ether organic solvents residues in leather and its products. The recovery of this method was 81.1% ~ 95.9%, and the relative standard deviation (RSD, n = 9) was 1.4% ~ 9.6%. Under the condition of signal to noise ratio (S / N) of 10, the lower limit of quantification (LOQ) of each component was 0.05 ~ 0.20mg / kg. The method has the advantages of simple operation, quick and convenient operation, high sensitivity, and can meet the technical requirements of detecting residues of ethylene glycol ether organic solvents in leather and its products, and provides a reference for formulating relevant testing standards.