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目的建立黄酒和醋中塑化剂的液液萃取-气相色谱-质谱联用法(GC-MS)快速检测技术。方法通过对不同提取液的比较,选择以乙酸乙酯-正己烷为提取液,采用HP-5MS色谱柱进行程序升温和分离测定,以内标法定量测定本地市售的13种黄酒和34种醋中17种邻苯二甲酸酯的含量。结果在本实验条件下,17种塑化剂的分离效果较好,当质量浓度的线性范围为0.10 mg/L~1.00 mg/L时,相关系数(r)为0.990~0.999,标准曲线的线性关系良好。17种PAEs的检出限除BMEP、DEEP、BBP的检出限为0.05 mg/kg外,其他均为0.025 mg/kg。黄酒中17种PAEs的回收率和RSD分别为74.7%~102.7%和2.7%~7.9%,醋中的回收率和RSD分别为70.0%~96.0%和2.5%~9.3%。结论该方法操作简单、可靠,可用于黄酒和醋中多种邻苯二甲酸酯类化合物的快速确证与定量检测。
Objective To establish a liquid-liquid extraction-gas chromatography-mass spectrometry (GC-MS) rapid detection technique for plasticizers of rice wine and vinegar. Methods Based on the comparison of different extracts, the ethyl acetate-n-hexane was chosen as the extraction solution, and the temperature and separation were determined by HP-5MS column. The domestic standard 13 kinds of rice wine and 34 kinds of vinegar In 17 kinds of phthalate content. Results Under the experimental conditions, the separation efficiency of 17 plasticizers was better. The correlation coefficient (r) was 0.990 ~ 0.999 when the linear range of mass concentration was 0.10 mg / L ~ 1.00 mg / L. The linearity Good relationship. The detection limits of 17 kinds of PAEs except for the detection limit of BMEP, DEEP, BBP were 0.05 mg / kg, the other were 0.025 mg / kg. The recoveries and RSDs of 17 PAEs in rice wine were 74.7% ~ 102.7% and 2.7% ~ 7.9%, respectively. The recoveries and RSDs were 70.0% ~ 96.0% and 2.5% ~ 9.3%, respectively. Conclusion The method is simple and reliable and can be used for the rapid confirmation and quantitative detection of many phthalates in rice wine and vinegar.