中国中药杂志

2019, v.44(23) 5083-5087

[打印本页] [关闭]
本期目录(Current Issue) | 过刊浏览(Past Issue) | 高级检索(Advanced Search)

免疫亲和柱净化光化学衍生高效液相色谱-荧光检测法同时测定土鳖虫中黄曲霉毒素B_1,B_2,G_1,G_2,M_1,M_2
Simultaneous determination of aflatoxin B_1,B_2,G_1,G_2,M_1,M_2 in Eupolyphaga Steleophaga by immunoaffinity column clean-up and HPLC-FLD with post-column photochemical derivatization

于鹏浩;张磊;秦家安;王建华;杨世海;杨美华;
YU Peng-hao;ZHANG Lei;QIN Jia-an;WANG Jian-hua;YANG Shi-hai;YANG Mei-hua;College of Traditional Chinese Medicine,Jilin Agricultural University;Institute of Medicinal Plant Development,Chinese Academy of Medical Sciences and Peking Union Medical College;College of Agronomy,Shandong Agricultural University;

摘要(Abstract):

通过建立免疫亲和柱净化光化学衍生高效液相色谱-荧光检测法测定土鳖虫中黄曲霉毒素B_1,B_2,G_1,G_2,M_1,M_2的污染情况。采用Cloversil C_(18)色谱柱(4. 6 mm×250 mm,5μm)进行分离,以甲醇-乙腈-水(20∶20∶60)为流动相,等度洗脱,荧光检测器激发波长360 nm,发射波长450 nm,流速0. 8 m L·min-1,色谱柱温度30℃。样品通过免疫亲和柱净化后,在上述色谱条件下,呈现良好的回收率,回收率为75. 47%~101. 8%,RSD均低于6. 7%。共检测土鳖虫样品20批次,根据《中国药典》2015年版一部中黄曲霉毒素B_1限量小于5μg·kg-1,黄曲霉毒素总量(黄曲霉毒素B_1,B_2,G_1,G_2)不超过10μg·kg~(-1)作为参考,有10批次样品检出为阳性,检出率为50. 0%,7批次样品超标,超标样品占阳性样品的比率高达70. 0%。其中有3批次样品同时检出含有黄曲霉毒素B_1,B2,G_1,G_2,M_1,M_2(SD-1,AH-1,AH-3),有1批次检出含有黄曲霉毒素B_1,B_2,G_1,G_2,M_1(AH-7)。实验结果表明,此方法适用于土鳖虫中6种黄曲霉毒素的同时检测,且提示对于其易污染黄曲霉毒素情况应高度重视。
The contamination of aflatoxin B_1,B_2,G_1,G_2,M_1 and M_2 in Eupolyphaga Steleophaga was determined by immunoaffinity column clean-up and HPLC-FLD with post-column photochemical derivatization. Chromatographic separations were carried out using a Cloversil C_(18) column( 4. 6 mm×250 mm,5 μm) that were eluted in isocratic with methanol-acetonitrile-water( 20 ∶ 20 ∶ 60) as the mobile phase. The excitation wavelength and the emission wavelength of fluorescence detector were maintained at 360 nm and 450 nm,respectively. The flow rate was 0. 8 m L·min~(-1),and the column temperature was 30 ℃ . The sample was prepared using the immunoaffinity column,then the recovery was measured with 75. 47%-101. 8% with RSD values lower than 6. 7%. A total of 20 batches of Eupolyphaga Steleophaga samples were assayed. According to the Chinese Pharmacopoeia( 2015 edition,part 1),the aflatoxin B_1 limit should be less than 5 μg·kg~(-1),and the sum of aflatoxins( AFB_1,AFB2,AFG_1,AFG_2) should be less than 10 μg·kg-1. Therefore,the positive rate of the 20 samples was 50. 0%,and 7 batches of samples exceeded the standard,and the over-standard rate was as high as 70. 0%. Among them,aflatoxins B_1,B_2,G_1,G_2,M_1,and M_2 were detected in three batches( SD-1,AH-1,AH-3),and aflatoxins B_1,B2,G1,G2,and M1 were detected in one batch( AH-7). The results showed that the newly developed method in this work is suitable for the simultaneous determination of six aflatoxins in Eupolyphaga Steleophaga,and also suggested that it should be of high values to take the contamination with aflatoxins into concerns.

关键词(KeyWords): 黄曲霉毒素;土鳖虫;免疫亲和柱;高效液相色谱;荧光检测器
aflatoxin;Eupolyphaga Steleophaga;immunoaffinity column;HPLC;fluorescence detector

Abstract:

Keywords:

基金项目(Foundation): 国家自然科学基金项目(81872999);; 中国医学科学院医学与健康科技创新工程项目(2017-I2M-1-013);; 国家重点研发计划项目(2016YFE0112900);; 国家级外专项目(G20190001631)

作者(Author): 于鹏浩;张磊;秦家安;王建华;杨世海;杨美华;
YU Peng-hao;ZHANG Lei;QIN Jia-an;WANG Jian-hua;YANG Shi-hai;YANG Mei-hua;College of Traditional Chinese Medicine,Jilin Agricultural University;Institute of Medicinal Plant Development,Chinese Academy of Medical Sciences and Peking Union Medical College;College of Agronomy,Shandong Agricultural University;

Email:

DOI:

参考文献(References):

扩展功能
本文信息
服务与反馈
本文关键词相关文章
本文作者相关文章
中国知网
分享