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采用液液萃取和超高效液相色谱-串联质谱法分析非酒精啤酒中的黄曲霉毒素。

Analysis of aflatoxins in nonalcoholic beer using liquid-liquid extraction and ultraperformance LC-MS/MS.

机构信息

Advanced Materials Research Chair, Department of Chemistry, College of Science, King Saud University, Riyadh, Kingdom of Saudi Arabia.

出版信息

J Sep Sci. 2013 Feb;36(3):572-7. doi: 10.1002/jssc.201200752. Epub 2012 Dec 4.

DOI:10.1002/jssc.201200752
PMID:23212744
Abstract

Aflatoxins AFB1, AFB2, AFG1, and AFG2 are toxic secondary metabolites produced by Aspergillus flavus and Aspergillus parasiticus and posses a potential threat to food safety. In the present work, liquid-liquid extraction and ultraperformance LC-MS/MS method has been applied for the determination of four naturally occurring aflatoxins AFB1, AFB2, AFG1, and AFG2 in nonalcoholic beer. Aflatoxins extraction from nonalcoholic beer was carried out using liquid-liquid extraction procedure. The effects of solvent-types were studied to obtain maximum recovery of the target analytes with minimum contamination. Among different solvents, the aflatoxins extraction was best achieved using ethyl acetate. The obtained recoveries were ranged from 85 to 96% with good quality parameters: LOD values between 0.001 and 0.003 ng/mL, linearity of the calibration curve (r(2) > 0.999), and repeatability (run-to-run) and reproducibility (day-to-day) precisions with RSDs lower than 5% (n = 5) achieved at 0.50 ng/mL concentration. The optimized liquid-liquid extraction in combination with ultraperformance LC-MS/MS was applied successfully to the analysis of AFB1, AFB2, AFG1, and AFG2 aflatoxins in 11 nonalcoholic beers and were detected up to 15.31 ng/L in some of the samples.

摘要

黄曲霉毒素 AFB1、AFB2、AFG1 和 AFG2 是黄曲霉和寄生曲霉产生的有毒次生代谢物,对食品安全构成潜在威胁。本工作采用液-液萃取和超高效液相色谱-串联质谱法测定非酒精啤酒中的四种天然黄曲霉毒素 AFB1、AFB2、AFG1 和 AFG2。采用液-液萃取法从非酒精啤酒中提取黄曲霉毒素。研究了溶剂类型的影响,以获得目标分析物的最大回收和最小污染。在不同的溶剂中,使用乙酸乙酯可以最好地提取黄曲霉毒素。回收率在 85%至 96%之间,具有良好的质量参数:LOD 值在 0.001 至 0.003ng/mL 之间,校准曲线的线性(r(2)>0.999),以及在 0.50ng/mL 浓度下重复性(运行间)和重现性(日间)精度的 RSD 低于 5%(n=5)。优化的液-液萃取与超高效液相色谱-串联质谱联用成功应用于 11 种非酒精啤酒中 AFB1、AFB2、AFG1 和 AFG2 黄曲霉毒素的分析,在一些样品中检测到高达 15.31ng/L。

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