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低成本腐殖酸键合硅胶作为一种有效的固相萃取吸附剂,用于食用油中黄曲霉毒素的简便测定。

Low-cost humic acid-bonded silica as an effective solid-phase extraction sorbent for convenient determination of aflatoxins in edible oils.

机构信息

Guangxi Zhuang Autonomous Region Center for Disease Prevention and Control, Nanning, Guangxi 530028, PR China.

School of Pharmaceutical Science, Guangxi Medical University, Nanning, Guangxi 530021, PR China.

出版信息

Anal Chim Acta. 2017 Jun 1;970:38-46. doi: 10.1016/j.aca.2017.02.029. Epub 2017 Mar 29.


DOI:10.1016/j.aca.2017.02.029
PMID:28433057
Abstract

Aflatoxins (AFs) are highly toxic, mutagenic, carcinogenic, and teratogenic secondary metabolites produced by the toxigenic fungi Aspergillus flavus and Aspergillus parasiticus. AFs tend to contaminate a wide range of foods which is a serious and recurring food safety problem worldwide. Currently, immunoaffinity chromatography (IAC) has become the most conventional sample clean-up method for determining AFs in foodstuffs. However, IAC method is limited in the large-scale food analysis because it requires the use of expensive disposable cartridges and the IA procedure is time-consuming. Herein, to achieve the cost-effective determination of AFs in edible oils, we developed a promising solid-phase extraction (SPE) method based on commercially available humic acid-bonded silica (HAS) sorbent, followed by high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS) analysis. In HAS-SPE, AFs can be captured by the HAS sorbent with both hydrophobic and hydrophilic interactions, whereas the oil matrix was captured only with the hydrophobic interactions. The oil matrix can be sufficiently washed off with isopropanol, while the AFs were still retained on the SPE packing, thus achieving selective extraction of AFs and clean-up of oil matrices. Under the optimal conditions of HAS-SPE, satisfactory recoveries ranging from 82% to 106% for four AFs (B, B, G, and G) were achieved in various oil matrices, containing blended oil, tea oil, rapeseed oil, peanut oil, sunflower seed oil, corn oil, blended olive oil, rice oil, soybean oil, and sesame oil. Only minor matrix effects ranging from 99% to 105% for four AFs were observed. Moreover, the LODs of AFs between 0.012 and 0.035 μg/kg completely meet the regulatory levels fixed by the EU, China or other countries. The methodology was further validated for assaying the naturally contaminated peanut oils, and consistent results between the HAS-SPE and the referenced IAC were obtained. In addition, HAS-SPE can directly treat diluted oil sample without liquid-liquid extraction and is automatable, thus making it simple and convenient for the large-scale determination of AFs in edible oils. Using this method, we successfully detected four AFs in the naturally contaminated peanut oils, which is, to the best of our knowledge, the first report about the determination of AFs in edible oils using HA-based SPE.

摘要

黄曲霉毒素(AFs)是由产毒真菌黄曲霉和寄生曲霉产生的剧毒、致突变、致癌和致畸的次生代谢物。AFs 往往会污染广泛的食品,这是一个全球性的严重且反复出现的食品安全问题。目前,免疫亲和色谱(IAC)已成为测定食品中 AFs 的最常规的样品净化方法。然而,由于需要使用昂贵的一次性筒和 IA 程序耗时,因此 IAC 方法在大规模食品分析中受到限制。在此,为了实现食用油脂中 AFs 的经济高效测定,我们开发了一种基于市售腐殖酸键合硅胶(HAS)吸附剂的有前途的固相萃取(SPE)方法,随后进行高效液相色谱串联质谱(HPLC-MS/MS)分析。在 HAS-SPE 中,AFs 可以通过 HAS 吸附剂与疏水性和亲水性相互作用来捕获,而油基质仅通过疏水性相互作用来捕获。油基质可以用异丙醇充分冲洗掉,而 AFs 仍保留在 SPE 填料上,从而实现 AFs 的选择性提取和油基质的净化。在 HAS-SPE 的最佳条件下,在各种油基质中(包括混合油、茶籽油、菜籽油、花生油、葵花籽油、玉米油、混合橄榄油、米糠油、大豆油和芝麻油),四种 AFs(B1、B2、G1 和 G2)的回收率在 82%至 106%之间,结果令人满意。对于四种 AFs,仅观察到 99%至 105%的小基质效应。此外,AFs 的检测限(LOD)在 0.012 至 0.035μg/kg 之间,完全符合欧盟、中国或其他国家规定的监管水平。该方法进一步用于测定天然污染的花生油,HAS-SPE 和参考 IAC 之间的结果一致。此外,HAS-SPE 可以直接处理稀释的油样,无需液液萃取,并且可以自动化,因此便于对食用油中的 AFs 进行大规模测定。使用这种方法,我们成功地检测到天然污染的花生油中的四种 AFs,据我们所知,这是首次使用基于 HA 的 SPE 测定食用油中 AFs 的报告。

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[7]
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[8]
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