传统补酒中邻苯二甲酸酯类化合物测定方法的优化及产生原因的分析

Optimization of detection method for phthalate acid esters in traditional tonic wine and analysis of its causes

建立了传统补酒中十八种邻苯二甲酸酯类化合物的气相色谱-质谱测定法,所建方法各目标化合物在各自浓度范围内线性良好,相关系数均大于0.9990,方法定量限0.025 mg/kg或者0.125 mg/kg,比国标方法规定的定量限0.3 mg/kg^9.0 mg/kg降低了许多。仪器精密度0.8%~3.4%,对于黄酒基传统补酒的加标回收率93.8%~108.8%,相对标准偏差0.2%~5.6%,对于白酒基传统补酒,加标回收率84.3%~111.3%,相对标准偏差0.3%~8.6%。本方法对于传统补酒企业的内部质量控制起到了重要的作用。同时,对该企业全品类传统补酒成品及关键原料进行了分析,找到了传统补酒中邻苯二甲酸二正丁酯(DBP)偏高的原因,是生产设备内衬高分子材料引起的,建议全部改用食品级不锈钢设备。

The detection method of GC-MS for 18 kinds of phthalate acid esters in traditional tonic wine was established.The linear range of the target compounds was good and the correlation coefficients were all greater than 0. 9990. The quantitative limit of the method was 0. 025 mg/kg or 0. 125 mg/kg,much lower than the limit of 0. 3 mg/kg - 9. 0 mg/kg stipulated by the national standard method. The relative standard deviation（ RSD） for instrument precision was between0. 8% and 3. 4%. The recovery of traditional yellow rice tonic wine was between 93. 8% and 108. 8%,RSD was between0. 2% and 5. 6%. The recovery of traditional liquor tonic wine was between 84. 3% and 111. 3%,RSD was between0. 3% and 8. 6%. The method played an important role in internal quality control for traditional tonic wine enterprises. At the same time,all kinds of traditional tonic wine products and key raw materials were detected and analyzed. It was found that the high DBP content in traditional tonic wine was caused by the lining polymer material in the production equipment.It was suggested that all stainless steel equipment of food grade should be used instead.