固相萃取–液相色谱–荧光检测法测定半夏中 苯并[a]芘残留量

Determination of benzo[a]pyrene residues in Pinellia ternata using solid phase extraction and liquid chromatography with fluorescence detection

中文关键词:  固相萃取  液相色谱-荧光检测法  半夏  苯并[a]芘  中药材

英文关键词:solid phase extraction  liquid chromatography with fluorescence detection  Pinellia ternate  benzo[a]pyrene  Chinese herbal medicine

中文摘要:

      目的 建立半夏样品中苯并[a]芘残留量的固相萃取-液相色谱-荧光检测法。方法 样品用水浸泡后, 用正己烷萃取, 硅胶固相萃取柱和ENV固相萃取柱净化, 分析时采用SUPELCOSILTM LC-PAH(25 cm×4.6 mm, 5 μm)色谱柱分离, 以乙腈-水(85:15=V:V)为流动相, 荧光检测激发波长384 nm, 发射波长406 nm, 外标法定量。结果 苯并[a]芘的检出限为0.1 μg/kg, 在1.0~50.0 ng/mL浓度范围内, 苯并[a]芘的线性相关系数为0.9999, 线性关系良好, 方法回收率在78.0%~102.5%范围内, 相对标准偏差低于9.6%。结论 该方法准确、实用、简便、快速, 在中药材的苯并[a]芘残留量检测方面有广泛应用前景。

英文摘要:

      Objective To establish a method for the determination of benzo[a]pyrene residues in Pinellia ternata by solid phase extraction and liquid chromatography with fluorescence detection method. Methods The samples were soaked with water and extracted with n-hexane, then cleaned up with silica gel solid phase extraction column and ENV solid phase extraction column. The sample was performed on a SUPELCOSILTM LC-PAH (25 cm×4.6 mm, 5 μm) column by using mobile phase acetonitrile/water 85:15 (V:V). A fluorescence detector was operated at excitation/emission wavelength 384/406 nm. Quantitation analysis was carried out with the external standard method. Results The detection limit of benzo[a]pyrene was 0.1 μg/kg and the correlation coefficient had a linearity in the range of 1.0~50.0 ng/mL (r=0.9999). The recoveries ranged from 78.0% to 102.5% with relative standard deviations less than 9.6%. Conclusion The method is accurate, practical, simple and fast, and has extensive application prospect for determination of benzo[a]pyrene residues in Chinese herbal medicine.