液相微萃取-HPLC法测定复杂样品中的双酚A

Determination of BPA in Complex Samples by Liquid Phase Microextraction Coupled with High Performance Liquid Chromatography

目的研究不同包装的牛奶、矿泉水以及购物小票等复杂样品中双酚A（BPA）的富集和测定。方法采用两相中空纤维（HF）液相微萃取（LPME）技术结合高效液相色谱（HPLC）法测定BPA,优化萃取剂、样品溶液p H值、萃取温度、萃取时间、搅拌速率以及Na Cl浓度等LPME参数,获得BPA的富集倍数和线性方程。结果确定了最优化的LPME条件,以正辛醇为萃取剂,样品溶液p H值为6.2,萃取温度为40℃,萃取时间为40 min,搅拌速率为500 r/min,不加盐调节;线性方程为y=590.03x＋39.98,相关系数r=0.9997,检测限为12.7μg/L,相对标准偏差（RSD）为4.2%,且BPA的富集倍数可达205倍,平均回收率达90.0%~105.0%。结论该方法大大提高了检测的灵敏度和选择性,用于实际样品分析时,结果稳定、可靠。

The aim of this study was to investigate the enrichment and detection of bisphenol A（BPA） in complex samples, such as milk with different packages, mineral water and receipts. BPA was detected using hollow-fiber（HF）two-phase liquid phase microextraction（LPME） coupled with high performance liquid chromatography（HPLC）. LPME parameters such as the extractant, the p H of the sample solution, the extraction temperature, the stirring rate, the extraction time and the concentration of Na Cl were optimized, and then the enrichment factor and the linear equation of BPA were obtained. The optimum conditions of LPME were as follows： n-octyl alcohol as extractant, p H 6.2 of sample solution,extraction temperature of 40℃, extraction time of 40 min, 500 r/min stirring rate and no Na Cl added to sample solution. The linear equation was y=590.03x＋39.98, with a correlation coefficient（r） of 0.9997, the limit of detection was 12.7 μg/L and the relative standard deviation was 4.2%. The enrichment factor of BPA reached 205 times, and the average recoveries rate was within the range of 90.0% ~105.0%. This method had higher sensitivity and selectivity. When it was applied to the determination of actual samples, the results were stable and reliable.