在线凝胶色谱-气相色谱-质谱法快速测定白酒中 邻苯二甲酸酯的含量

Rapid determination of phthalate acid esters in liquor by on-line gel permeation chromatography-gas chromatography-mass spectrometry

中文关键词:  白酒  邻苯二甲酸酯  凝胶色谱  气相色谱-质谱法

英文关键词:liquor  phthalate acid esters  gel permeation chromatography  gas chromatography-mass spectrometry

中文摘要:

      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(r2≥0.9909), 方法检出限为0.7~2.8 μg/L, 定量限为2.3~9.2 μg/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。

英文摘要:

      Objective To establish a method for determination of phthalate acid esters (PAEs) in liquor by on-line gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC-MS). Methods Without pretreatment, the liquor sample was analyzed by GPC-GC-MS for its content of PAEs after being mixed. Results There were good linear relationships between the peak areas of PAEs and their corresponding concentration which ranged from 0.10 mg/L to 10.0 mg/L with correlation coefficients not less than 0.9909. The limits of detection of method were 0.7~2.8 μg/L, the limits of quantification were 2.3~9.2 μg/L, and the average recoveries of PAEs ranged from 80.4% to 95.6% at 3 different spiked levels with the relative standard deviations were between 1.5% and 6.5%. Conclusion This method is simple, quick, and has low risks of plasticizer contamination, high automation, accuracy, precision and sensitivity, which is suitable for the rapid analysis of PAEs in liquor.