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目的采用在线凝胶色谱-气相色谱-质谱(gel permeation chromatography-gas chromatography-mass spectrometry,GPC-GC-MS)检测方法测定白酒中的邻苯二甲酸酯类物质(phthalate acid esters,PAEs)。方法白酒样品不经前处理,混匀后采用在线GPC-GC-MS直接进样分析其中的PAEs含量。结果在0.10~10.0 mg/L范围内,PAEs的峰面积与浓度间的线性关系良好(r~2≥0.9909),方法检出限为0.7~2.8μg/L,定量限为2.3~9.2μg/L;在0.10、1.0、10.0 mg/mL 3个添加水平下,PAEs的平均回收率为80.4%~95.6%,相对标准偏差为1.5%~6.5%。结论本方法简单、快速、塑化剂污染风险低、自动化程度较高,且准确度、精密度和高灵敏度较高,适用于白酒中PAEs的快速分析检测。
OBJECTIVE To determine the content of phthalate acid esters (PAEs) in liquor by on-line gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC-MS) Methods The samples of liquor were not pretreated and the contents of PAEs were directly analyzed by on-line GPC-GC-MS after mixing. The results showed that the linear relationship between the concentration of PAEs peak area and concentration was good (r ~ 2≥0.9909) in the range of 0.10 ~ 10.0 mg / L, the detection limit was 0.7 ~ 2.8μg / L, the limit of quantification was 2.3 ~ 9.2μg / L. The average PAEs recoveries ranged from 80.4% to 95.6% with relative standard deviations from 1.5% to 6.5% at the three levels of 0.10, 1.0 and 10.0 mg / mL. Conclusion The method is simple and rapid, with low risk of plasticizer contamination, high degree of automation, and high accuracy, precision and high sensitivity. It is suitable for the rapid analysis and detection of PAEs in liquor.