摘要
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 Gas chromatography - mass spectrometry （ GC - MS） with the internal standard quantitative determina- tion was developed for the determination of 17 phthalate acid esters（PAEs） in rice wine and vinegar after liquid - liquid extrac- tion. Methods According to the comparison, the ethyl acetate/hexane solution was selected as the extracting solution, with which the content of 17 PAEs in samples （locally produced 13 kinds of rice wine and 34 kinds of vinegar） were detected and quantified with internal standard after temperature programming and isolation on a HP -5MS column. Results The separation effect of 17 phthalate acid esters could be good under the lab conditions. When the linear range were among 0. 10 mg/L - 1.00 mg/L, the correlation coefficients（r） were greater than 0. 990, with good linearity of standard curve. The detection limit of 17 PAEs, except BMEP, DEEP, BBP, was 0.05 mg/kg, and the others were all 0.025 mg/kg. Recoveries of rice wine and vinegar were in the range of 74.7% -102.7% and 70.0% -96.0%, respectively, with relative standard deviations （RSD） of 2.7% - 7.9% and 2.5 % -9.3 %, respectively. Conclusion It is a simple and reliable method, which can be applied for the rapid detection and confirmation of PAEs in rice wine and vinegar samples.
出处
《中国卫生检验杂志》
CAS
2015年第22期3842-3845,共4页
Chinese Journal of Health Laboratory Technology
基金
镇江市科技支撑计划(社会发展)项目(SH2013066)
