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建立了测定白酒中6种邻苯二甲酸酯类增塑剂的真空离心浓缩/气相色谱-质谱联用(GC-MS)分析方法。样品经真空离心浓缩,正己烷提取,取上层正己烷,4000r/min离心5min,采用GC-MS测定,外标法定量。在0.10～5.00μg/mL范围内,相关系数r2>0.992,样品在0.10～2.00 mg/kg范围内加标,平均回收率在88.83%～111.67%之间,相对标准偏差(RSD)为4.85%～11.35%,检出限(LOD)在0.02～0.05 mg/kg之间。采用该方法对16个白酒样品进行测定,结果表明该法简便、快速、结果准确可靠、灵敏度高,能够满足白酒中6种邻苯二甲酸酯增塑剂检测需求。
A vacuum centrifugation concentration-gas chromatography-mass spectrometry (GC-MS) method for the determination of six phthalate plasticizers in liquor was established. Samples were concentrated by vacuum centrifugation, hexane extraction, the upper layer of n-hexane, 4000r / min centrifugation 5min, using GC-MS, external standard. The correlation coefficient r2> 0.992 in the range of 0.10 ~ 5.00μg / mL. The average recoveries ranged from 88.83% to 111.67%. The relative standard deviations (RSDs) were 4.85% ~ 11.35%, the detection limit (LOD) was between 0.02 ~ 0.05 mg / kg. The method was applied to the determination of 16 liquor samples. The results showed that the method was simple, rapid, accurate, reliable and sensitive. It could meet the detection requirements of six kinds of phthalate plasticizers in liquor.