响应面法优化养殖水体中炔雌醇的固相萃取条件

Optimization of Solid-phase Extraction Conditions for Ethinylestradiol in Aquaculture Water by Response Surface Method

在单因素试验、Plackett-Burman设计试验基础上,采用Box-Behnken响应面法对养殖水体中炔雌醇(EE2)的固相萃取条件进行优化。结果表明,洗脱液体积、洗脱液组成和淋洗液体积是影响EE2固相萃取回收率的3个主要因素;EE2的最佳固相萃取条件为:水样pH值为3,进样流量为3.0 mL/min,淋洗液为体积分数为10%的甲醇水溶液,淋洗液体积7.0 mL,洗脱液为乙酸乙酯-正己烷混合溶液(体积比为9∶1),洗脱液体积12.0 mL。该条件下养殖水样中EE2固相萃取回收率为81.6%~86.7%。

On the basis of single factor experiment and Plackett-Burman design,the solid phase extraction conditions for ethinylestradiol(EE2)in aquaculture water were optimized by response surface method(Box-Behnken Design).The results showed that the volume and composition of the eluant,the volume of the leacheate were the three main factors affecting the recoveries of EE2 extraction.The optimum conditions of SPE were as follows:pH value of water sample was 3,the injection flow rate was 3.0 mL/min,the leacheate was methanol solution of 10%volume fraction,the leacheate volume was 7.0 mL,the eluent was ethyl acetate-n-hexane mixed solution(volume ratio 9∶1),the eluent volume was 12.0 mL.Under these conditions,the recoveries of EE2 in aquaculture water samples were 81.6%~86.7%.