高效液相色谱-荧光检测法分析 100 种食品和药用植物中的玉米赤霉烯酮和α-玉米赤霉烯醇及液相色谱-串联质谱法阳性确证
Analysis of zearalenone and α-zearalenol in 100 foods and medicinal plants determined by HPLC-FLD and positive confirmation by LC-MS-MS.
机构信息
Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences, Peking Union Medical College, Beijing, 100193, China.
出版信息
J Sci Food Agric. 2013 May;93(7):1584-90. doi: 10.1002/jsfa.5926. Epub 2012 Oct 24.
BACKGROUND
Mycotoxins, which may contaminate many foods and medicinal plants, are poisonous to humans. A high-performance liquid chromatography with fluorescence detection (HPLC-FLD) method was successfully developed for analysing the contamination levels of zearalenone (ZON) and its metabolite α-zearalenol (α-ZOL) in 100 widely consumed foods and medicinal plants in China. Samples were extracted with methanol-water (80:20, v/v), and cleaned up by using an immunoaffinity column.
RESULTS
The limits of detection of this developed method for ZON and α-ZOL were 4 µg kg(-1) and 2.5 µg kg(-1) , respectively. Recoveries for the samples spiked with three levels (30, 60 and 300 µg kg(-1) for ZON and α-ZOL) ranged from 85.8% to 96.1% with relative standard deviation (RSD) of 2.6-7.1% for ZON, and from 89.9% to 98.7% with RSD of 1.9-9.2% for α-ZOL. Twelve (12%) of these tested samples were contaminated with ZON at levels ranging from 5.3 to 295.8 µg kg(-1). The most contaminated samples were Semen coicis, four of them in a concentration level exceeding 60 µg kg(-1) 'maximum level' (range 68.9-119.6 µg kg(-1)). Positive samples were further confirmed by liquid chromatography-tandem mass spectrometry.
CONCLUSION
The results suggest that it is necessary to control ZON contamination in medicinal plants, especially Semen coicis. This is a successful study on the analysis of ZON and α-ZOL in medicinal plants in China by HPLC-FLD. Immunoaffinity clean-up and HPLC-FLD proved to have broad applicability in the field of simultaneously detecting ZON and α-ZOL in foods and medicinal plants and other complicated matrices.
背景
真菌毒素可能会污染许多食物和药用植物,对人类有毒。本研究成功建立了一种高效液相色谱-荧光检测法(HPLC-FLD),用于分析中国 100 种常见食用食物和药用植物中玉米赤霉烯酮(ZON)及其代谢物α-玉米赤霉烯醇(α-ZOL)的污染水平。样品用甲醇-水(80:20,v/v)提取,用免疫亲和柱净化。
结果
该方法检测 ZON 和 α-ZOL 的检出限分别为 4 µg kg(-1) 和 2.5 µg kg(-1)。ZON 和 α-ZOL 三种添加水平(30、60 和 300 µg kg(-1))的回收率在 85.8%至 96.1%之间,相对标准偏差(RSD)为 2.6-7.1%;在 89.9%至 98.7%之间,RSD 为 1.9-9.2%。在这些检测的样品中,有 12 种(12%)被 ZON 污染,含量范围为 5.3 至 295.8 µg kg(-1)。污染最严重的样品是薏苡仁,其中 4 种样品的浓度超过了 60 µg kg(-1)的“最大限量”(范围为 68.9-119.6 µg kg(-1))。阳性样品进一步通过液相色谱-串联质谱法进行了确认。
结论
该研究结果表明,有必要控制药用植物,特别是薏苡仁中 ZON 的污染。这是在中国首次成功地用 HPLC-FLD 分析药用植物中的 ZON 和 α-ZOL。免疫亲和净化和 HPLC-FLD 证明在同时检测食物和药用植物及其他复杂基质中的 ZON 和 α-ZOL 方面具有广泛的适用性。