Wang Xia, Diao Chun-Peng, Zhao Ru-Song
Key Laboratory for Applied Technology of Sophisticated Analytical Instruments of Shandong Province, Analysis and Test Center, Shandong Academy of Sciences, Jinan, Shandong, China.
J Sep Sci. 2009 Jan;32(1):154-9. doi: 10.1002/jssc.200800436.
This paper described a novel approach for the determination of bisphenol A by dispersive liquid-phase microextraction with in situ acetylation prior to GC-MS. In this derivatization/extraction method, 500 microL acetone (disperser solvent) containing 30.0 microL chlorobenzene (extraction solvent) and 30.0 microL acetic anhydride (derivatization reagent) was rapidly injected into 5.00 mL aqueous sample containing bisphenol A and K2CO3 (0.5% w/v). Within a few seconds the analyte was derivatized and extracted at the same time. After centrifugation, 1.0 microL of sedimented phase containing enriched analyte was determined by GC-MS. Some important parameters, such as type and volume of extraction and disperser solvent, volume of acetic anhydride, derivatization and extraction time, amount of K2CO3, and salt addition were studied and optimized. Under the optimum conditions, the LOD and the LOQ were 0.01, 0.1 microg/L, respectively. The experimental results indicated that there was linearity over the range 0.1-50 microg/L with coefficient of correlation 0.9997, and good reproducibility with RSD 3.8% (n = 5). The proposed method has been applied for the analysis of drinking water samples, and satisfactory results were achieved.
本文描述了一种在气相色谱-质谱联用（GC-MS）之前，通过原位乙酰化分散液液微萃取法测定双酚A的新方法。在这种衍生化/萃取方法中，将含有30.0微升氯苯（萃取溶剂）和30.0微升乙酸酐（衍生化试剂）的500微升丙酮（分散剂溶剂）迅速注入含有双酚A和碳酸钾（0.5% w/v）的5.00毫升水样中。在几秒钟内，分析物同时被衍生化和萃取。离心后，通过GC-MS测定1.0微升含有富集分析物的沉淀相。研究并优化了一些重要参数，如萃取和分散剂溶剂的类型和体积、乙酸酐的体积、衍生化和萃取时间、碳酸钾的量以及盐的添加量。在最佳条件下，检测限（LOD）和定量限（LOQ）分别为0.01、0.1微克/升。实验结果表明，在0.1-50微克/升范围内呈线性，相关系数为0.9997，相对标准偏差（RSD）为3.8%（n = 5），具有良好的重现性。该方法已应用于饮用水样品的分析，并取得了满意的结果。
