摘要: |
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pH值、 萃取温度、 萃取时间、 搅拌速率以及NaCl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 pH 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 12.7 μg/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。 |
关键词: 中空纤维 液相微萃取 双酚A 高效液相色谱 |
DOI: |
分类号:TS207 |
基金项目:江西省科技计划 (20133BBG70105) |
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Determination of BPA in Complex Samples by Liquid Phase Microextraction Coupled with High Performance Liquid Chromatography |
CAO Bo1, DING Jian-hua2,3, MIAO Pei-pei1, ZHANG Xiao-fen4, LIN Hai-lu1
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1.East China Institute of Technology, Nanchang 330013, China;2.1. East China Institute of Technology, Nanchang 330013, China;3.2. Fudan University, Shanghai 200433, China;4.Pingyang Drainage Co., Ltd., Pingyang 325401, China
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Abstract: |
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 pH of the sample solution, the extraction temperature, the stirring rate, the extraction time and the concentration of NaCl 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, pH 6.2 of sample solution, extraction temperature of 40 ℃, extraction time of 40 min, 500 r/min stirring rate and no NaCl 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. |
Key words: hollow fiber liquid-phase microextraction bisphenol A high performance liquid chromatography |