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

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,5μm)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0.1μg/kg,在1.0~50.0 ng/m L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。

ABSTRACT:Objective To establish a method for the determination of benzo[a]pyrene residues inPinellia ternata by solid phase extraction and liquid chromatography with fluorescence detection method.Methods The samples were soaked with water and extracted withn-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, 5μm) 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 0.1μg/kg and the cor-relation 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, prac-tical, simple and fast, and has extensive application prospect for determination of benzo[a]pyrene residues in Chinese herbal medicine.