气相色谱-质谱法/同位素内标法测定白酒中16种邻苯二甲酸酯的优化研究

参照国家标准GB 5009.271—2016《食品安全国家标准食品中邻苯二甲酸酯的测定》中的方法，对气相色谱及质谱条件进行优化，并利用与气相色谱仪匹配的自动液体进样器自动添加内标，对白酒中的16种邻苯二甲酸酯进行测定。结果表明，条件优化后能使白酒中16种邻苯二甲酸酯得到较好的分离，在一定质量浓度范围内（0.02～0.20 mg/L），16种邻苯二甲酸酯具有良好的线性关系，R2≥0.998。邻苯二甲酸二正丁酯（DBP）的定量检出限为6.6×10-3 mg/kg，其余15种均小于3.0×10-2 mg/kg，平均回收率为88.6%～106.1%，相对标准偏差（RSD）为1.6%～4.3%。优化条件后，能够节省内标使用量，并且具有较高的准确度和灵敏度，能够满足上述国标对白酒中邻苯二甲酸酯检测的要求。

Optimization of the determination of 16 phthalate acid esters in Baijiu by GC-MS/Isotope internal standard method

Based on the National Standard GB 5009.271-2016 "Food Safety Standards, Determination of phthalate esters in food", the gas chromatography and mass spectrometry conditions of the method were optimized, and the internal standard was added by the automatic liquid sampler matched with GC, to detect 16 phthalate acid esters in Baijiu. The results showed that 16 phthalate acid esters in Baijiu were separated well under the optimized conditions, and had a good linear relationship within 0.02-0.20 mg/L, with correlation coefficient R2≥0.998. The di-n-butyl phthalate quantification limit was 6.6×10-3 mg/kg, the others were less than 3.0×10-2 mg/kg. Their average recoveries varied from 88.6% to 106.1% and the relative standard deviations (RSD) ranged from 1.6% to 4.3%. The method could save the application amount of isotope internal standard, and had high accuracy and sensitivity under the optimized conditions. It could satisfy the national standard for the phthalate acid esters detection in Baijiu.