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
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摘要: 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。Abstract: 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. 61mol/L, the pH of Na2HPO4-NaH2PO4 buffer solution was 7.09, and the volume of EDTA-Fe (Ⅱ) and H2O2 was 0.55mL, 1.63mL respectively. Snail samples were ultrasonic extracted by hexane and dichloromethane 1∶1 mixed 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.
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