荧光法测定贝类邻苯二甲酸酯总量的条件优化

Optimization of fluorimetry for determination phthalate esters in snails by response surface methodology

为准确检测贝类邻苯二甲酸酯(PAEs)总量,通过响应面法优化荧光法测定样品中PAEs的条件。探讨了不同NaOH浓度,缓冲溶液pH,EDTA-Fe(Ⅱ)和H2O2用量对PAEs在Fenton反应体系中产生荧光强度的影响。经响应面优化的最佳荧光反应条件如下:NaOH溶液的浓度为4.61mol/L,缓冲溶液的pH为7.09,EDTA-Fe(Ⅱ)和H2O2溶液的加入量分别为0.55和1.63mL。螺蛳样品采用正己烷与二氯甲烷1∶1混合溶液按1∶1.6的固液比超声振荡萃取后在优化条件下测定PAEs总量,方法的相对标准偏差为1.73%～6.56%,加标回收率为93.80%～106.11%,所检测螺蛳中PAEs含量达26.64～44.89mg/kg。

The optimum conditions for determining total phthalate esters（PAEs） in snail samples by fluorimetry were established by using response surface methodology（ RSM）.The optimal levels were as follows：the concentration of NaOH was 4.61 mol/L, the pH of Na2 HPO4- Nail2 PO4 buffer solution was 7.09, and the volume of EDTA- Fe （II ） and H2O2 was 0.55mL, 1.63 mL respectively.Snail samples were ultrasonic extracted by hexane and dichloromethane 1：1mixed solution with 1：1.6 （g/mL）ratio of solid-to-liquid at first, and then were performed under the optimized conditions as mentioned above.The results showed that the relative standard deviation of the method were 1.73% 6.56%,the average recoveries ranged from 93.80% to 106.11%, and the PAEs of snail was about 26.64 44.89mg/kg.