反相液相色谱法测定膏状香精中邻苯二甲酸酯类
Determination of phthalate plasticizers in cream essence by reverse phase liquid chromatography
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摘要: 采用反相液相色谱法研究了膏状香精中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二正丁基酯(DBP)、邻苯二甲酸丁基苄基酯(BBP)4种邻苯二甲酸酯的萃取条件。利用正交实验对影响萃取总量的3个主要因素(正己烷用量、超声时间、水浴温度)进行了优化,确定了萃取的最佳条件:正己烷用量10mL,超声时间25min,水浴温度15℃。结果表明,该分析条件下,样品猪骨膏、牛肉膏的加标回收率为90%94%。用乙腈-水等梯度洗脱(75∶25),4种PAEs分离较好,在0.520mg/L之间,色谱峰面积与4种邻苯二甲酸酯的浓度呈现良好的线性关系。Abstract: Four phthalate acid esters in cream essence, such as dimethyl phthalate (DMP) , diethyl phthalate (DEP) , dibutyl phthalate (DBP) and benzyl butyl phthalate (BBP) , were determined by reverse phase liquid chromatography. The conditions for extraction were researched. Orthogonal design experiment was carried out to optimize the 3 dominant factors (hexane volume, ultrasonic time, water temperature) affecting extraction recovery. The optimum conditions for solid phase extraction were determined as follows:hexane volume 10mL, ultrasonic time 25min, water temperature 15℃. Results showed that the recoveries of the four phthalates were 90%94%.There was a good linear relationship between peak area and concentration of 4 phthalate esters in range of 0.520mg/L.