磁性介孔沸石復(fù)合材料對花生樣品中黃曲霉毒素B₁的快速富集

摘要： 本研究通過改性沸石介孔性能的方法制備新型吸附材料磁性介孔沸石，利用磁性分散固相萃取結(jié)合高效液相色譜法，建立了花生中黃曲霉毒素B₁ （AFB₁）的提取方法。通過場發(fā)射掃描電子顯微鏡、傅立葉變換紅外光譜、比表面積和磁性分析技術(shù)分析材料理化性質(zhì)。結(jié)果顯示，磁性介孔沸石復(fù)合材料Fe₃O₄/zeolite-b雜質(zhì)更少、孔洞更多、內(nèi)徑更大且孔道結(jié)構(gòu)更加明顯，并且孔徑大小集中、平均孔徑較大，具有超強(qiáng)磁性；將磁性介孔沸石材料作為吸附劑，通過優(yōu)化萃取條件，結(jié)合高效液相色譜-熒光檢測器檢測花生樣品中的AFB₁。結(jié)果表明，當(dāng)磁性介孔沸石的添加量為25 mg，pH為7，樣品體積為1.0 mL，吸附時間為1 min，洗脫劑為乙腈，洗脫劑體積為3 mL，洗脫時間為3 min時，AFB₁質(zhì)量濃度為2.00～20.00 μg/L，目標(biāo)物色譜峰面積與質(zhì)量濃度有良好的線性關(guān)系，決定系數(shù)（R²）為0.976 8，方法檢測限0.05 μg/L，定量限0.16 μg/L。3種不同加標(biāo)質(zhì)量濃度（2.00 μg/L、10.00 μg/L、20.00 μg/L）下，AFB₁加標(biāo)回收率范圍為81.3%～92.6%，相對標(biāo)準(zhǔn)偏差為2.2%～3.4%。

關(guān)鍵詞： 磁性固相萃取；介孔沸石；黃曲霉毒素；花生

中圖分類號： TQ424

文獻(xiàn)標(biāo)識碼： A

文章編號： 1000-4440（2024）11-2177-10

Rapid enrichment of magnetic mesoporous zeolite composites on aflatoxin B₁ in peanut samples

HUANG Jing¹， WANG Wenting¹， ZHANG Chushu²， ZHOU Haixiang²， WANG Mian²， TANG Yueyi²， ZHU Lifei²， ZHANG Jiancheng²

（1.Liaoning Technical University， Fuxin 123000， China;2.Shandong Peanut Research Institute， Qingdao 266000， China）

Abstract： In this study， a new adsorption material magnetic mesoporous zeolite was prepared by modifying the mesoporous properties of zeolite. The extraction method of aflatoxin B₁ （AFB₁） from peanut was established by magnetic dispersion solid phase extraction combined with high performance liquid chromatography. The physical and chemical properties of the materials were analyzed by field emission scanning electron microscopy （FE-SEM）， Fourier transform infrared spectroscopy （FT-IR）， Brunauer-Emmett-Teller （BET） and hysteresis loop （VSM）. The results showed that Fe₃O₄/zeolite-b composite materials had less impurities， more holes， larger inner diameter and more obvious pore structure， and the pore size was concentrated， the average pore size was larger， which had super magnetic properties. The magnetic mesoporous zeolite material was used as adsorbent to detect AFB₁ in peanut samples by optimizing extraction conditions and combining with high performance liquid chromatography-fluorescence detector （FD）. The results showed that the mass concentration of AFB₁ was 2.00-20.00 μg/L when the addition amount of magnetic mesoporous zeolite was 25 mg， the pH was seven， the sample volume was 1.0 mL， the extraction time was 1 min， the elution agent was acetonitrile， the elution volume was 3 mL， the adsorption time was 3 min， and the chromatographic peak area of the target object had a good linear relationship with the mass concentration. The coefficient of determination （R²） was 0.976 8， the detection limit was 0.05 μg/L， and the quantitation limit was 0.16 μg/L. Under three different mass concentrations （2.00 μg/L， 10.00 μg/L， 20.00 μg/L）， the recoveries of AFB₁ were 81.3%-92.6%， and the relative standard deviations were 2.2%-3.4%.

Key words： magnetic solid phase extraction;mesoporous zeolite;aflatoxin;peanut

黃曲霉毒素（AFs）主要是由黃曲霉和寄生曲霉等曲霉菌產(chǎn)生的真菌毒素，是一類具有較強(qiáng)毒性和致癌性的雙呋喃環(huán)類毒素^[1-3]。通常情況下，AFs會污染儲存中的飼料和糧食，對人和動物的健康以及食品安全構(gòu)成威脅^[4-5]。目前已發(fā)現(xiàn)約有 20 種不同種類的黃曲霉毒素，其中黃曲霉毒素B₁（AFB₁）分布最廣、含量最高、毒性最強(qiáng)^[6]。至今超過75個國家立法規(guī)定了AFB₁的限量標(biāo)準(zhǔn)，中國食品中AFB₁的限量標(biāo)準(zhǔn)為0.5～20.0 μg/kg，嬰兒配方食品中為0.5 μg/kg，花生中為20.0 μg/kg。……