摘要
采用免疫亲和柱净化-光化学柱后衍生-高效液相色谱法测定中药材柏子仁中的黄曲霉毒素G_2、G_1、B_2和B_1。样品经甲醇(7+3)溶液提取,提取液经免疫亲和柱净化,用甲醇洗脱,洗脱液经黄曲霉毒素专用C18色谱柱分离,以甲醇(45+55)溶液为流动相进行洗脱,柱后光化学衍生波长为254nm,荧光检测器的激发波长为365nm,发射波长为440nm。黄曲霉毒素G2、B2的线性范围均为0.125~5.0μg·L^(-1),黄曲霉毒素G_1、B_1的线性范围均为0.50~20μg·L^(-1),检出限(3S/N)在0.012~0.047μg·L^(-1)之间。加标回收率81.4%~105%之间,测定值的相对标准偏差(n=6)在1.6%~6.9%之间。
A method of HPLC combined with immunoaffinity column cleanup and post-column photochemical derivatization was applied to determine aflatoxins G_2,G_1,B_2 and B_1 in platycladi seeds,which was a kind of Chinese herbal medicine.The sample was extracted with methanol（7＋3）solution,then the extraction was purified by immunoaffinity column and the analyte was eluted by methanol.The eluent was separated on a special C_（18） chromatographic column for aflatoxins with a methanol（45＋55）solution as mobile phase.The wavelength of postcolumn photochemical derivatization was 254 nm,and the excitation wavelength and emission wavelength of fluorenscence detector were 365 nm and 440 nm,respectively.The linearity ranges of aflatoxins G_2 and B_2 were both0.125-5.0μg·L-1,and the linearity ranges of aflatoxins G_1 and B_1 were both 0.50-20μg·L-1,with detection limits（3S/N）in the range of 0.012-0.047μg·L-1.Recovery rates obtained by standard addition method were in the range of 81.4%-1 05% and RSDs（n=6）were in the range of 1.6%-6.9%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2016年第5期541-544,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
2015年度河南省重点科技攻关项目(152102310130)
2015年河南职业技术学院科研基金项目(2015HZK05)
关键词
高效液相色谱法
黄曲霉毒素
柏子仁
免疫亲和柱
光化学衍生
HPLC
Aflatoxins
Platycladi seeds
Immunoaffinity column cleanup
Photochemical derivatization
