超声辅助溶剂棒微萃取-液相色谱法快速测定婴儿配方奶粉中的双酚A
Rapid determination of bisphenol A in infant formula milk powder by ultrasound-assisted solvent bar microextraction coupled with high performance liquid chromatography
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摘要: 建立超声辅助溶剂棒微萃取-高效液相色谱(UA-SBME-HPLC)方法,用于快速测定婴儿配方奶粉中的双酚A(BPA)。设计超声辅助溶剂棒微萃取系统,优化后的最佳萃取条件为:溶剂棒的有效长度为30 mm,萃取溶剂为正辛醇,搅拌速度为600 r/min,超声时间10 min,萃取时间15 min,pH=6的HCl溶液为给体相,0.12 mol/L NaOH溶液为受体相,NaCl的加入浓度为60 g/L。在最优萃取条件下,该方法对BPA的平均富集倍数为102倍,方法的线性范围为0.1100μg/L(r=0.9989),检出限为0.35μg/L(S/N=3),相对标准偏差RSD小于4.32%(n=6),加标回收率为89.7%102.8%。研究表明该方法绿色环保,可用于准确快速测定婴儿配方奶粉中的双酚A。Abstract: A technique for the rapid determination of bisphenol-A ( BPA) in infant formula milk powder was developed by ultrasound-assisted solvent bar microextraction coupled with high performance liquid chromatography.The system of ultrasound-assisted solvent bar microextraction was designed. The optimized microextraction conditions were as follows: the length of solvent bar was 30 mm, 1-octanol was used as the extraction solvent, the stirring rate was 600 r/min, the ultrasonic time was 10 min and the extraction time was 15 min, the pH of sample solutions was 6, 0.12 mol/L of NaOH was used as the acceptor phase, the concentration of NaCl was 60 g/L. Under the optimal microextraction conditions, the average enrichment factor was102, the linear range was 0.1 ~ 100 μg/L ( r = 0.9989) , the limits of detection was 0.35 μg/L ( S/N = 3) , and the relative standard deviations ( RSD) was lower than 4.32% ( n = 6) . The proposed method was applied to the determination of BPA in infant formula milk powder samples.The spiked recoveries were in the range of 89.7% 102.8%.It was showed that the proposed method was environmentally for the rapid determination of BPA in infant formula milk powder.