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
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。
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.
标题：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
英文标题：Determination of benzo[a]pyrene residues in Pinellia ternata using solid phase extraction and liquid chromatography with fluorescence detection
作者：
何强 陕西出入境检验检疫局
张璐 陕西出入境检验检疫局
李莹 陕西出入境检验检疫局
孔祥虹 陕西出入境检验检疫局
李建华 陕西出入境检验检疫局
邹阳 陕西出入境检验检疫局
付骋宇 陕西出入境检验检疫局
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,
发表日期：2015-10-26
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