盛装散装白酒的塑料桶中邻苯二甲酸二丁酯的测定

Determination of dibutyl phthalate in plastic bucket containing bulk liquor

据调查,农村市场广泛使用塑料桶盛装散装白酒。以正己烷作为提取溶剂,采用超声波辅助提取盛装散装白酒的塑料桶中邻苯二甲酸二丁酯(DBP),高效液相(HPLC)测定其含量。以提取时间、料液比、提取温度进行单因素实验,采用响应曲面Box-Behnken设计分析方法对其最佳提取条件进行优化。结果表明,邻苯二甲酸二丁酯最佳的提取条件为:提取时间为52min、料液比为1∶40、提取温度为49℃,在此条件下,DBP提取量为32.21mg/kg,与理论预测值基本吻合。在0.5～50.0mg/L范围内邻苯二甲酸二丁酯具有良好的线性关系(R2=0.9998),最低检出限0.017mg/L;标准品精密度实验的相对标准偏差为0.40%,邻苯二甲酸二丁酯的回收率为99.68%及相对标准偏差为0.85%,结果表明,该提取方法准确可靠,为食品的安全性和增塑剂的风险性评估提供了基础数据。

According to the survey that rural market to hold bulk liquor extensively use of plastic bucket. Hexane was used to extraction solvent,extract dibutyl phthalate（DBP） from the plastic buckets containing bulk liquor by ultrasound-assisted extraction as well as dibutyl phthalate quantification was performed by high performance liquid chromatography（HPLC）. Extraction time,material/liquid ratio and extraction temperature were investigated with single-factor test. Response surface methodology based on Box-Behnken experimental desigen was used for process optimization. The optimal extraction conditions determined were extraction time of 52min, material/liquid ratio of 1：40,extraction temperature of 49℃. Under these conditions,the extraction volume of DBP was up to 32.21mg/kg,which was consistent with the prediction value. In the scope of 0.5~50.0mg/L, dibutyl phthalate had good linear relationship（R2=0.9998）,lowest detectable limit was 0.017mg/L. The relative standard deviation of standard experimental precision was 0.40%,the recovery of dibutyl phthalate was 99.68% and the relative standard deviation was 0.85% ,the result showed that this extract method was accurate and reliable. This provided the basic data for food safety and the risk assessment of plasticizer.