Diethylstilbestrol in Fish Tissue Determined Through Subcritical Fluid Extraction and with GC-MS  

作　　者：QIAO Qinghui SHI Nianrong FENG Xiaomei LU Jie HAN Yuqian XUE Changhu 

机构地区：[1]College of Food Science and Engineering, Ocean University of China

出　　处：《Journal of Ocean University of China》2016年第3期489-494,共6页中国海洋大学学报（英文版）

基　　金：supported by the National Natural Science Foundation of China (31071541);a program for Changjiang Scholars and Innovative Research Team in University (IRT1188)

摘　　要：As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more efficient technologies. Taking economic and environmental concerns into account, subcritical fluid extraction as a faster and more efficient method has stood out as a sample pre-treatment technology. This new extraction technology can overcome the shortcomings of supercritical fluid and achieve higher extraction efficiency at relatively low pressures and temperatures. In this experiment, a simple, sensitive and efficient method has been developed for the determination of diethylstilbestrol(DES) in fish tissue using subcritical 1,1,1,2-tetrafluoroethane(R134a) extraction in combination with gas chromatography-mass spectrometry(GC-MS). After extraction, freezing-lipid filtration was utilized to remove fatty co-extract. Further purification steps were performed with C_(18) and NH_2 solid phase extraction(SPE). Finally, the analyte was derived by heptafluorobutyric anhydride(HFBA), followed by GC-MS analysis. Response surface methodology(RSM) was employed to optimizing the extraction condition, and the optimized was as follows: extraction pressure, 4.3 MPa; extraction temperature, 26℃; amount of co-solvent volume, 4.7 m L. Under this condition, at a spiked level of 1, 5, 10 μg kg^(-1), the mean recovery of DES was more than 90% with relative standard deviations(RSDs) less than 10%. Finally, the developed method has been successfully used to analyzing the real samples.As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists＇ attention all over the world, and the development trend of sample preparation forwarded to faster and more efficient technologies. Taking economic and environmental concerns into account, subcritical fluid extraction as a faster and more efficient method has stood out as a sample pre-treatment technology. This new extraction technology can overcome the shortcomings of supercritical fluid and achieve higher extraction efficiency at relatively low pressures and temperatures. In this experiment, a simple, sensitive and efficient method has been developed for the determination of diethylstilbestrol（DES） in fish tissue using subcritical 1,1,1,2-tetrafluoroethane（R134a） extraction in combination with gas chromatography-mass spectrometry（GC-MS）. After extraction, freezing-lipid filtration was utilized to remove fatty co-extract. Further purification steps were performed with C_（18） and NH_2 solid phase extraction（SPE）. Finally, the analyte was derived by heptafluorobutyric anhydride（HFBA）, followed by GC-MS analysis. Response surface methodology（RSM） was employed to optimizing the extraction condition, and the optimized was as follows： extraction pressure, 4.3 MPa; extraction temperature, 26℃; amount of co-solvent volume, 4.7 m L. Under this condition, at a spiked level of 1, 5, 10 μg kg-1, the mean recovery of DES was more than 90% with relative standard deviations（RSDs） less than 10%. Finally, the developed method has been successfully used to analyzing the real samples.

关 键 词：subcritical R134a extraction DIETHYLSTILBESTROL GC-MS determination fish tissue 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]