CAJ | 학술논문

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SUPELCOSILTMLC-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/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。
목적：건립반하양품중분병[a]비잔류량적고상췌취-액상색보-형광검측법。방법양품용수침포후,용정기완췌취,규효고상췌취주화ENV고상췌취주정화,분석시채용SUPELCOSILTMLC-PAH(25 cm×4.6 mm,5μm)색보주분리,이을정-수(85：15=V：V)위류동상,형광검측격발파장384 nm,발사파장406 nm,외표법정량。결과분병[a]비적검출한위0.1μg/kg,재1.0~50.0 ng/mL농도범위내,분병[a]비적선성상관계수위0.9999,선성관계량호,방법회수솔재78.0%~102.5%범위내,상대표준편차저우9.6%。결론해방법준학、실용、간편、쾌속,재중약재적분병[a]비잔류량검측방면유엄범응용전경。
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.