化学计量学优化-分散液液微萃取-荧光分析法测定食品接触物中双酚A的迁移量  

Determination of the migration of bisphenol a from food contacted materials by chemometrics optimized dispersive liquid-liquid microextraction with fluorescence spectrophotometry

作　　者：方鸽[1] 张加玲[1] 王彤[1] 王松[1] 

机构地区：[1]山西医科大学公共卫生学院,太原030001

出　　处：《分析试验室》2012年第10期96-100,共5页Chinese Journal of Analysis Laboratory

基　　金：山西医科大学科技创新基金资助(02100906)资助

摘　　要：建立了分散液液微萃取-荧光分析法测定双酚A的方法,并对塑料水杯和塑料袋中双酚A的迁移量进行测定。经Plackett-Burman设计筛选影响因素后,利用中心复合表面设计确定了最佳萃取条件。利用全因子设计确定荧光测定条件为:0.2 mol/L HCl,4×10-4mol/Lβ-环糊精。在水、10%乙醇条件下,方法线性范围1～50μg/L(r=0.999),检出限为0.53μg/L;在3%乙酸条件下,线性范围为1～60μg/L(r=0.997),检出限为0.85μg/L。方法回收率为95.4%～111.2%,相对标准偏差(n=6)为13%～16%。所测样品在室温水中双酚A迁移量低于检出限,在沸水、3%乙酸及10%乙醇中均有不同程度迁移。An analytical method, dispersive liquid-liquid mieroextraction-fluorescence spectrophotometry, was developed for the determination of the migration amount of bisphenol A （BPA） from food contacted materials. An appropriate mixture of chlorobenzene and acetone was injected rapidly into the sample and as a result cloudy mixture was formed. After centrifugation, the water phase was thrown away. The mixture of solvent for the determination was added into the centrifugal tube after dried the chlorobenzene. The optimal extraction conditions of 5 mL of water sample volume, 40 μL of extraction solvent （chlorobenzene）, 1 mL of disperser solvent （acetone）, extraction time of 1 min, pH value of 6, centrifugation speed of 3500 r/min, centrifugation of 5 mintime were obtained by central composite face-centered design （CCF）. The optimal determination conditions of 0. 2 mol/L HCL, 2 × 10-4 mol/L β-cyclodextrin were achieved by full factorial design. Under the optimum conditions, the calibration graph was linear in the range of 1 -50μg/L（ R = 0. 999） in the water and 10% ethanol. The limit of detection was 0. 53 μg/L. The calibration graph was linear in the range of 1 -60 μg/L（ R =0. 997） in the 3% acetic acid. The limit of detection was 0.85μg/L. The recoveries ranged from 95.4% to 111.2%, while the relative standard deviation （RSD） were 13% - 16% （n = 6）. The bisphenol A has different migration amounts in boiling water, 3% acetic acid and 10% ethanol. The migration amount was lower than the detection limit in the water of normal temperature. The developed method was environmentally benign, rapid, simple and low cost for the determination of the migration amount of bisphenol A .

关 键 词：化学计量学 分散液液微萃取 荧光分析法 双酚A 迁移量 

分 类 号：O652[理学—分析化学] O657.3[理学—化学]