摘要
对白酒塑化剂检测过程样品的前处理方法进行选择与优化,考察了酒中乙醇除去方式、进样方式、提取溶剂种类对塑化剂检测的样品前处理影响,并分别采用直接提取、水浴氮吹、净化小柱、固相萃取四种不同的前处理方法,分别考察方法的回收率、精密度、检出限.结果表明,气相色谱-质谱联用法（GC-MS）测定白酒中邻苯二甲酸二丁酯（DBP）、邻苯二甲酸二（2-乙基）己酯（DEHP）、邻苯二甲酸二异壬酯（DINP）的样品前处理较优方法为水浴氮吹去除乙醇、正己烷与乙酸乙酯（比例4：1）为溶剂,采取萃取进样方式.该法在0.5～10.0 μg/mL范围内DBP、DEHP、DINP线性良好,线性相关系数分别为0.998、0.994、0.977.方法的检出限为0.05 mg/kg,添加量为0.05 mg/kg、0.50 mg/kg、1.00 mg/kg时,平均回收率为95.82％～107.26％,相对标准偏差RSD为2.84％～8.36％（n=6）.
The pretreatment method of Chinese liquor samples for phthalate （a plasticizer） detection was selected and optmized.The effect of different ethanol removal ways,sampling method,extraction solvent type on pretreatment was investigated.Adopting direct extraction,water bath nitrogen blow,purification and solid phase extraction method respectively for pretreatment,the recovery rate,precision,detection limit of the four methods were detected.The results showed that the optimal pretreatment method for determination of dibutyl phthalate （DBP）,di-2-ethyl hexyl phthalate （DEHP）,diisononyl phthalate （DINP） in liquor by GC-MS was water bath nitrogen removal of ethanol,n-hexane and ethyl acetate （4∶1） as the solvent to conduct sample extraction.The calibration curves of method showed good linearity in the range of 0.5-10.0 μg/ml to determinate DBP,DEHP and DINP in Chinese liquor.Linear correlation coefficient was 0.998,0.994,0.977,respectively.The detection limit was 0.05 mg/kg.When the addition was 0.05 mg/kg,0.50 mg/kg,1.00 mg/kg,the average recovery ranged from 95.82％ to 107.26％,and the relative standard deviation was between 2.84％ and 8.36％ （n=6）.
出处
《中国酿造》
CAS
北大核心
2015年第1期137-142,共6页
China Brewing
基金
湖南省科技厅科技计划项目(2013FJ6092)
邵阳学院研究生科研创新项目(CX2013SY002)
