基于磁性固相萃取的赭曲霉毒素A检测方法构建及优化  

Construction and Optimization of a Detection Method for OTA Based on Magnetic Solid Phase Extraction

作　　者：王丙辰 王逸凡 张秀媛 何扩 WANG Bingchen;WANG Yifan;ZHANG Xiuyuan;HE Kuo(Hebei Key Laboratory of Quality&Safety Analysis-testing for Agro-products and Food,Hebei North University,Zhangjiakou 075000,Hebei,China)

机构地区：[1]河北北方学院河北省农产品食品质量安全分析检测重点实验室,河北张家口075000

出　　处：《食品研究与开发》2025年第4期162-168,共7页Food Research and Development

摘　　要：为实现对葡萄酒中赭曲霉毒素A(ochratoxin A,OTA)的定量检测,使用具有三层核壳结构的磁性金属有机框架(metal-organic framework,MOF)材料对葡萄酒中的目标毒素进行磁固相萃取,并结合高效液相色谱法构建一种操作便捷、特异性强、灵敏度高的检测方法。以GB 5009.96—2016《食品安全国家标准食品中赭曲霉毒素A的测定》为基础,对试验过程进行优化,得到最佳前处理条件。结果表明,在反应溶液为中性、磁性MOF材料用量为0.8 mg时可在10 min内达到最大吸附效率,随后使用2 mL洗脱液(乙腈+1.5%甲酸)洗脱6 min达到最大洗脱效率。在上述条件下,OTA的检测质量浓度在0.05~10.00 ng/mL时线性关系良好(R~2=0.998 5)。当加标量为0.06 ng/mL时,测定值的相对标准偏差(n=3)为3.32%,回收率为95.83%;当加标量为0.10 ng/mL时,测定值的相对标准偏差为2.09%,回收率为96.70%;当加标量为0.20 ng/mL时,测定值的相对标准偏差为2.51%,回收率为101.5%。该方法操作简便、特异性强,通过对OTA的快速磁分离-富集可有效避免共存元素的影响并提高测定的灵敏度。To achieve the quantitative determination of ochratoxin A(OTA)in wine,a magnetic metal-organic framework(MOF)material with a three-layer core-shell structure was used for magnetic solid phase extraction of the target toxin from the wine.Combined with high-performance liquid chromatography,a simple,specific,and highly sensitive detection method for OTA in wine was developed.Based on GB 5009.96—2016 Determi-nation of Ochratoxin A in Food Safety National Standard,the experimental process was optimized to obtain the best pretreatment conditions.The results showed that the maximum adsorption efficiency was achieved within 10 min when the reaction solution was neutral and the amount of magnetic MOF material was 0.8 mg.Following this,the maximum elution efficiency was achieved at the 6 min using 2 mL of eluent(acetonitrile+1.5%formic acid).Under these conditions,the detection of OTA showed a good linear relationship in the range of 0.05 to 10.00 ng/mL(R2=0.9985).At a spiked concentration of 0.06 ng/mL,the relative standard deviation of the measurements(n=3)was 3.32%,and the recovery rate was 95.83%.At a spiked concentration of 0.10 ng/mL,the relative standard deviation was 2.09%and the recovery rate was 96.70%.At a spiked concentration of 0.20 ng/mL,the relative standard deviation was 2.51%and the recovery rate was 101.5%.This method was easy to operate and highly specific,effectively avoiding the influence of coexisting elements and improving the sensitivity of the determination through rapid magnetic separation and enrichment of OTA.

关 键 词：赭曲霉毒素A 纳米材料 金属有机框架 磁固相萃取 液相色谱法 

分 类 号：O657.72[理学—分析化学] TS262.6[理学—化学]