液-液微萃取结合气质联用法测定白酒中15种塑化剂含量

Determination of 15 plasticizer contents in Baijiu by liquid-liquid microextraction with gas chromatography-mass spectrometry

为考察白酒中塑化剂含量,采用表面活性剂强化乳化液-液微萃取结合气相色谱-质谱联用法测定32份不同白酒中15种邻苯二甲酸酯类塑化剂的含量。结果表明,该方法在0.008~5.00μg/mL范围内呈良好线性关系,15种塑化剂的最低检出限在1.44~1.50μg/L范围内,加标回收率在89.71%~117.73%之间,回收率试验结果相对标准偏差(RSD)范围为1.71%~6.82%,精密度试验结果RSD均<2.53%,重复性试验结果RSD均<3.60%,精密度、重复性良好,准确度高。在32份不同香型白酒样品中,9种塑化剂的检出率均>70%,其中邻苯二甲酸二乙酯的检出率100%,检出值范围为0.001~0.740μg/mL。主成分分析(PCA)结果表明,塑化剂含量与白酒香型相关性不显著(P>0.05),相关性分析结果表明塑化剂含量之间存在极显著相关性(P<0.01)。

To investigate the plasticizer content in Baijiu(Chinese liquor),the content of 15 kinds of phthalic acid esters plasticizers in 32 different Baijiu were determined by the surfactant enhanced emulsion liquid microextraction combined with GC-MS.The results showed that the linear range of the method was 0.008-5.00μg/ml,and the detection limits of 15 plasticizers were 1.44-1.50μg/L.The recoveries were 89.71%-117.73% with the relative standard deviation(RSD)of 1.71%-6.82%.The RSD of precision test result was less than 2.53%and the RSD of repeatability test result was less than 3.60%.The precision,accuracy and repeatability were good,and the recovery rate was high.In 32 different flavor Baijiu samples,the detection rates of 9 plasticizers were more than 70%,and the detection rates of diethyl phthalate was 100%.The detection value of diethyl phthalate was 0.001-0.740μg/ml.The principal component analysis(PCA)showed the correlation between plasticizer content and Baijiu flavor was not significant(P>0.05),and the correlation analysis showed that there was a highly significant correlation between plasticizers(P<0.01).