摘要
目的:采用免疫亲和净化HPLC柱后紫外光化学衍生荧光检测法研究中药饮片中黄曲霉毒素测定的加样回收率,考察该方法在中药饮片黄曲霉毒素残留测定中的可行性,评价120批中药饮片的污染状况,总结污染规律。方法:样品经溶剂提取、免疫亲和柱净化后由HPLC柱后光衍生荧光检测法测定其中黄曲霉毒素残留量,对每种饮片进行4μg.kg-1(以黄曲霉毒素B1计)的加样回收率考察。结果:黄曲霉毒素B1、B2、G1、G2的最低检测限分别为0.44,0.12,0.41,0.16 pg;线性范围分别为1.74～218.0,0.50～62.17,1.63～203.1,0.62～61.94 pg(r﹥0.9999)。所考察饮片中黄曲霉毒素B1、B2、G1、G2总回收率和B1回收率均在60%～120%之间的占87%;被污染的批次占9.2%,其中污染程度超过目前中国药典限度的占6.7%。结论:免疫亲和净化HPLC柱后光衍生荧光检测法具有方法简便,衍生反应稳定,灵敏度高,重现性好,反应系统污染少的优点,适合于大多数中药饮片的黄曲霉毒素检测;种子类被污染的程度严重,应扩大该类中药的监测范围。
Objective：To investigate the recoveries of aflatoxin（AF） residues analysis of traditional Chinese medi- cine （TCM） Yinpian using immunoaffinity column HPLC method with post column photochemical derivatization and fluorescence detection, and evaluate the feasibility of the method. To evaluate the contamination status of 120 bat- ches of TCM Yinpian and summarize the rule of contamination Methods ： Samples were prepared through organic solvent extraction and cleaned up with immunoaffinity column sequentially ; the recoveries of aflatoxins were then de- termined by adding aflatoxins standard mixture at the level of 4 μg·kg^-1 according to aflatoxin B1 content. Finally, aflatoxins Bl, B2, G1 and G2 residue amount in TCM Yinpian was determined. Results ：The limit of detection of aria- toxins Bl , B2, G1, G2 was 0. 44,0. 12,0.41,0. 16 pg, respectively; Aflatoxins B1, B2, G1, G2showed good linear rela- tionships at the ranges of 1.74 -218.0 pg,0.50 -62. 17 pg, 1.63 -203.1 pg and 0.62 -61.94 pg, respectively, r 〉 0. 9999. The recoveries of total aflatoxins and aflatoxin B~ in 87% detected samples were between 60% - 120% ~ 9.2% of TCM Yinpian was detected to be contaminated by aflatoxins,and aflatoxins amount in 6. 7% exceeded the limit of Chinese Pharmacopoeia of the People~ Republic of China 2010. Conclusion ：The method showed con- venient operation, stable derivation reaction, high sensitivity, good repeatability and little pollution, which meets the requirement of aflatoxin residues determination in most TCM Yinpian. The seeds are easy to be contaminated, so theaflatoxins control in those TCM should be expanded.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2012年第12期2203-2207,共5页
Chinese Journal of Pharmaceutical Analysis
基金
"十一五"国家科技支撑计划(2008BAI55B02)
大连市科技计划基金项目(2011E15SF121)
关键词
黄曲霉毒素
二呋喃香豆素类代谢产物
中药饮片毒性成分
高效液相色谱
光衍生
免疫亲和柱
回收率
安全监测
aflatoxins
difurocoumarines metabolites
prepared traditional Chinese medicine toxic ingredients
HPLC
photochemical derivation
immunoaffinity column
recovery
safety monitoring
