基于免疫亲和-高效液相色谱-柱后光化学衍生法的菊苣药材中黄曲霉毒素残留量研究

Study on Aflatoxin Residues in Chicory Based on Immunoaffinity-High Performance Liquid Chromatography-Post-Column Photochemical Derivation

目的:首次分析菊苣药材中黄曲霉毒素B_(1)、B_(2)、G_(1)、G_(2)的残留量,并对其安全性风险进行探讨,为菊苣药材质量评价提供数据支撑。方法:样品经匀浆处理后采用免疫亲和柱进行净化,以高效液相色谱-柱后光化学衍生法为检测方法,色谱柱为Venusil MP C_(18)柱(150 mm×4.6 mm,5μm),以甲醇-乙腈-水为流动相进行梯度洗脱,流速为1.0 ml·min^(-1),柱温为40℃,荧光检测器激发波长为360 nm,发射波长为450 nm。对收集的42批次菊苣地上部分及根进行分析,根据黄曲霉毒素的含量对其潜在的风险进行探讨。结果:黄曲霉毒素B_(1)、B_(2)、G_(1)、G_(2)检测方法的线性关系、精密度、回收率及重复性均较好。由测定结果可看出,所有批次的菊苣药材不同药用部位中,仅1批次菊苣地上部分检出黄曲霉毒素B_(1)和B_(2),其他批次药材均未检出,检出率为2.4%。参照中国药典2020年版黄曲霉毒素的限量标准,检出样品中黄曲霉毒素B_(1)残留量超标,总量同样超过限度规定。结论:菊苣药材黄曲霉毒素整体检出率较低,潜在的安全性风险较小。

Objective:To analyze the residues of aflatoxin B_(1),B_(2),G_(1) and G_(2) in chicory for the first time,and discuss the safety risk of aflatoxin,so as to provide data support for the quality evaluation of chicory.Methods:The samples were homogenized and purified on an immunoaffinity column using high performance liquid chromatograph-post-column photochemical derivatization method.The determination was performed on a Venusil MP C_(18)(150 mm×4.6 mm,5μm)column with methanol-acetonitrile-water as the mobile phase for gradient elution at the flow rate of 1.0 ml·min^(-1).The column temperature was 40℃.The excitation wavelength of the fluorescence detector was 360 nm and the emission wavelength was 450 nm.The aboveground parts and roots of 42 batches of chicory collected were analyzed,and the potential risks were discussed according to the content of aflatoxin.Results:The linear relationship,precision,recovery and reproducibility of aflatoxin B_(1),B_(2),G_(1) and G_(2) were good.The results showed that aflatoxin B_(1) and B_(2) were detected in the aboveground part of chicory in only one batch with a detection rate of 2.4%.Referred to the current aflatoxin limit standard described in Chinese Pharmacopoeia(2020 edition),the residual amount of aflatoxin B_(1) in the sample was found to exceed the standard,and the total amount also exceeded the limit.Conclusion:The overall detection rate of aflatoxin in chicory is low with mild potential safety risk.