作者： 周韩玲，廖勤俭，宋廷富，安明哲，李杨华，王 芳，郭 艳，王小琴，罗 珠
建立酿酒原料中10种真菌毒素的高效液相色谱-串联质谱（LC-MS/MS）检测方法。样品经84 %乙腈提取后，采用黄曲霉毒素免疫亲和柱净化、外标法定量4种黄曲霉毒素；使用多功能柱净化、同位素内标法定量样品中另外6种真菌毒素。结果表明，10种真菌毒素在各自的线性范围内线性关系良好，相关系数不低于0.998，10种化合物检出限为0.0022～1.79 μg/L，定量限为0.075～5.95 μg/L；加标回收率为61 %～116.2 %，相对标准偏差为0.88 %～8.61 %。该方法具有灵敏度高、稳定性好、定量准确的特点，适用于不同酿酒原料中多种真菌毒素的定量检测。 |
高效液相色谱-串联质谱； 酿酒原料； 真菌毒素； 多功能柱； 免疫亲和柱 |
Simultaneous Determination of 10 Kinds of Mycotoxins in Liquor-Making Raw Materials by HPLC-MS/MS
ZHOU Hanling,LIAO Qinjian,SONG Tingfu,AN Mingzhe,LI Yanghua,WANG Fang,GUO Yan, WANG Xiaoqin and LUO
Technology Center of Wuliangye Group Co. Ltd., Yibin, Sichuan 644007, China
A method for simultaneous determination of 10 kinds of mycotoxins in liquor-making raw materials by HPLC-MS/MS had been developed. The samples were extracted with 84 % acetonitrile. Four kinds of aflatoxins were quantified by external standard method with aflatoxin immunoaffinity column purification, and the other six mycotoxins were quantified by internal standard method with multi-functional column purification. The results showed that the 10 mycotoxins had a good linear relationship in their respective linear range with a correlation coefficient no less than 0.998. The detection limits of the 10 compounds were 0.0022 μg/L to 1.79 μg/L with the limits of quantitation as 0.075 μg/L to 5.95 μg/L. The recoveries were 61 % to 116.2 % with the relative standard deviations as 0.88 % to 8.61 %. This method had the advantages including high sensitivity, good stability and quantitative accuracy, and it was suitable for quantitative detection of various mycotoxins in different liquor-making raw materials.
high performance liquid chromatography-tandem mass spectrometry; liquor-making raw materials; mycotoxins; multifunctional column; immunoaffinity column