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Miniaturized vortex assisted-dispersive molecularly imprinted polymer micro-solid phase extraction and HPLC-MS/MS for assessing trace aflatoxins in cultured fish.
Analytical Methods ( IF 2.7 ) Pub Date : 2020-07-29 , DOI: 10.1039/d0ay01259a
G D Thilini Madurangika Jayasinghe 1 , Raquel Domínguez-González , Pilar Bermejo-Barrera , Antonio Moreda-Piñeiro
Affiliation  

A dispersive micro-solid phase extraction approach using a molecularly imprinted polymer as an adsorbent has been developed for pre-concentrating aflatoxins from cultured fish. Aflatoxins were first isolated from fish muscle and liver by an ultrasound assisted extraction procedure using a 60 : 40 acetonitrile/0.1 M KH2PO4 aqueous buffer (pH 6.0) mixture. Polymeric adsorbent beads were synthesized using 5,7-dimethoxycoumarin as a dummy template, methacrylic acid as a functional monomer, divinylbenzene as a crosslinker, and 2,2′-azobisisobutyronitrile as an initiator. Parameters affecting the steps of extraction procedure, including the sample (fish extract) pH, adsorption stirring speed and time, desorption stirring speed and time, elution solvent ratio, and polymer capacity, were investigated and optimized. The limit of detection was found to vary from 0.29 to 0.61 μg kg−1 for the several aflatoxins. The proposed method was shown to be accurate and precise. Intraday and inter-day relative standard deviations were lower than 20%, and intraday and inter-day analytical recoveries were within the 80–100% range. The prepared adsorbent in the dispersive micro-solid phase extraction format was re-usable, and the pre-concentration procedure was found to be simple, rapid and highly selective and sensitive to identify/quantify AFs in fish.

中文翻译:

微型涡旋辅助分散分子印迹聚合物微固相萃取和HPLC-MS / MS用于评估养殖鱼类中的痕量黄曲霉毒素。

已经开发了一种使用分子印迹聚合物作为吸附剂的分散微固相萃取方法,用于从养殖鱼中预浓缩黄曲霉毒素。首先使用60:40乙腈/0.1 M KH 2 PO 4通过超声辅助提取程序从鱼肌肉和肝脏中分离出黄曲霉毒素水性缓冲液(pH 6.0)混合物。使用5,7-二甲氧基香豆素作为虚拟模板,甲基丙烯酸作为功能单体,二乙烯基苯作为交联剂和2,2'-偶氮二异丁腈作为引发剂合成聚合物吸附剂珠。研究和优化了影响萃取程序步骤的参数,包括样品(鱼提取物)的pH,吸附搅拌速度和时间,脱附搅拌速度和时间,洗脱溶剂比和聚合物容量。发现检出限为0.29至0.61μgkg -1对于几种黄曲霉毒素。所提出的方法被证明是准确和精确的。日内和日间相对标准偏差低于20%,日内和日间分析回收率在80-100%范围内。所制备的分散微固相萃取形式的吸附剂可重复使用,并且预浓缩程序简单,快速,高度选择性且对鱼中AF的识别/定量非常敏感。
更新日期:2020-09-17
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