复合免疫亲和柱-高效液相色谱法同时测定谷物及其制品中9种真菌毒素

doi:10.3724/SP.J.1123.2018.08008

摘要/Abstract

摘要：

建立了复合免疫亲和柱-在线光化学衍生-高效液相色谱同时测定谷物及其制品中9种真菌毒素的检测方法。以乙腈-水（80：20，v/v）混合溶液提取样品中9种真菌毒素，提取液经自制真菌毒素复合免疫亲和柱净化，采用高效液相色谱进行分离，在线光化学衍生后进入荧光检测器测定，外标法定量。结果表明，9种真菌毒素在相应浓度范围内线性关系良好，相关系数均大于0.999；在低、中、高3个不同加标浓度下，9种真菌毒素的回收率均大于80%，相对标准偏差（RSD）为1.0%~5.6%；方法的检出限（LOD）为0.02~5.00 μg/kg，定量限（LOQ）为0.07~16.70 μg/kg。该方法具有重现性好、灵敏度高、结果准确的特点，适用于谷物及其制品中9种真菌毒素残留的分析检测。

关键词: 复合免疫亲和柱, 高效液相色谱法, 谷物及其制品, 真菌毒素

Abstract:

A rapid analytical method using high performance liquid chromatography (HPLC) with post-column derivatization was established for the simultaneous determination of nine mycotoxins in cereal and cereal products. The nine mycotoxins were extracted from the samples by using acetone-water (80:20, v/v). The extract was purified by a self-made composite immunoaffinity clean-up column and was analyzed by HPLC. Mycotoxins were detected by fluorescence detection after on-line photochemical derivatization and were quantified by an external standard method. The nine compounds showed good linearities in their concentration ranges with the correlation coefficients (R²) exceeding 0.999. The spiked recoveries in real samples for the nine mycotoxins were above 80%, while the relative standard deviations (RSDs) were in the range of 1.0%-5.6%. The limits of detection (LODs) and the limits of quantification (LOQs) were 0.02-5.00 and 0.07-16.70 μg/kg, respectively. The developed method is simple, sensitive, and has good repeatability, and thus can be used for the routine analysis of the nine mycotoxins in cereal and cereal products.

Key words: cereal and cereal products, composite immunoaffinity column, high performance liquid chromatography (HPLC), mycotoxin

中图分类号:

O658

王韦岗, 强敏, 端礼钦. 复合免疫亲和柱-高效液相色谱法同时测定谷物及其制品中9种真菌毒素[J]. 色谱, 2018, 36(12): 1330-1336.

WANG Weigang, QIANG Min, DUAN Liqin. Simultaneous determination of nine mycotoxins in cereal and cereal products by high performance liquid chromatography with composite immunoaffinity clean-up column[J]. Chinese Journal of Chromatography, 2018, 36(12): 1330-1336.

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