青稞酒中塑化剂测定方法研究及方法确认

Determination of Dibutyl Phthalate in Highland Barley Liquor

本试验建立了GC-MS法测定青稞酒中邻苯二甲酸二丁酯含量的方法。采用直接提取和平行蒸发除去乙醇,考察青稞酒中乙醇的含量对检测结果的影响。同时考察了该方法的准确度、精密度、回收率和检出限。试验结果表明,气相质谱法测定青稞酒中的邻苯二甲酸二丁酯的样品前处理方法为用平行蒸发仪除去乙醇,用正己烷为提取溶剂。该方法在邻苯二甲酸二丁酯含量为0.02~2.0μg/mL范围内线性良好,加标水平为0.1μg/mL、0.2μg/mL、1.0μg/mL 3个水平,其回收率为90.0%~102.0%,相对标准偏差为1.38%~3.18%,质控样品的z值比分为0.42,满足试验室质量控制要求。本方法前处理操作简单、快速、检测结果准确,重现性好,可用于青稞酒中邻苯二甲酸二丁酯的检测。

The determination method of dibutyl phthalate（DBP） in highland barley liquor by GC-MS had been developed. Direct extraction and parallel evaporation were adopted to remove ethanol in liquor sample pretreatment with n-hexane used as the extraction solvent. This method presented good linearity as DBP content was in the range of 0.02 μg/mL to 2.0 μg/mL. As the standard addition were at 0.1 μg/mL, 0.2 μg/mL and 1.0 μg/mL, the average recoveries ranged from 90.0 % to 102.0 %, the relative standard deviation was between 1.38 % to 3.18 %, and z-score of quality control samples was 0.42, which met lab requirements. This method had the advantages including simple pretreatment, rapid determination, accurate measurement, and good reproducibility, and it could be used to determine DBP in highland barley liquor.