摘要
建立了高效液相色谱法测定中药材阳春砂中黄曲霉素(AFT)B_1、B_2、G_1、G_2的方法。样品经提取、免疫亲和层析净化,采用荧光检测器,以柱后衍生系统结合HPLC检测。结果表明,阳春砂中4种黄曲霉素在1.00 μg/kg,10.00μg/kg和32.00 μg/kg 3个水平的加标回收率均在84.0%~101.0%之间,相对标准偏差均小于1.7%;方法最低检出限AFB1与AFG1为0.35 μg/kg,AFB2与AFG2为0.06 μg/kg;标准曲线良好,相关系数大于0.998 7。本方法可用于阳春砂中黄曲霉素的检验。
The paper is to present a quick and effective detection method for determining the aflatoxins B1, B2, Gl and (;2 in Chinese herbal medicine Amomum villosum. The samples of the herbal medicine we take as the case study were first extracted by using ace- tonitrile: water (9:1) and then cleaned-up by using an immuno-affini- ty colmnn with the analysis done by high performance liquid chro- matography (HPLC), including post-column derivatization for fluores- cence detection. While doing the experiments, we have also studied the optimal conditions for the extraction and chromatographic separa- tion, which was made possible to be finished in 10 min by adopting an isoeratic chromatographic system with a mobile phase comprising acetonitrile: methanol : water (7 : 28 : 65, V/ V/ V). In addition, we have made it possible for all the samples to recover each aflatoxin BI, B2, GI and G2 spiked to Amomum villosum at three levels of 1.00 μg/kg, 10.00 μg/kg and 32.00 μg/kg between 84.0%- 101.0% . With all the relative standard deviations made lower than 1.7 %, the lowest detection limits of aflatoxins in Chinese herbal medicine were 0.35 ~g/kg for AFB1 and AFG1, and 0.06 ~g/kg for AFB2 and AFG2. The calibration curves of all the above tested samples demon- strate perfect linearity with the correlation coefficient being 0.998 7. Thus, the method displays nice stability, high sensitivity and high selectivity, which suggests a great potential for the method to get extensively adopted for determining the aflatoxins in Amomum villosum. The results show that all the seven samples we have used were contaminated with aflatoxins, which ranges from 0.21 μg/kg to 4.92 μg/kg whereas the total aflatoxin levels in one sample proves to be beyond the standard limit of the European Union of 4 μg/kg.
出处
《安全与环境学报》
CAS
CSCD
北大核心
2010年第1期106-109,共4页
Journal of Safety and Environment
基金
广东省中医药管理局项目(2009277
1060008)