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采用液相色谱-串联质谱法测定橄榄油中的黄曲霉毒素

Determination of aflatoxins in olive oil by liquid chromatography-tandem mass spectrometry.

作者信息

Cavaliere Chiara, Foglia Patrizia, Guarino Chiara, Nazzari Manuela, Samperi Roberto, Laganà Aldo

机构信息

Department of Chemistry, Sapienza University of Rome, Piazzale Aldo Moro 5, 00185 Roma, Italy.

出版信息

Anal Chim Acta. 2007 Jul 16;596(1):141-8. doi: 10.1016/j.aca.2007.05.055. Epub 2007 Jun 3.

Abstract

A liquid chromatography-tandem mass spectrometric with electrospray ionization (LC/ESI-MS/MS) method for determining the four naturally occurring aflatoxins (AFs) B1, B2, G1, and G2 in olive oil is proposed. AFs were extracted from oil sample by means of matrix solid phase dispersion (MSPDE), utilizing C18 as dispersing material. No further purification step, such as lipid removal, was performed. Aflatoxin M1, the hepatic metabolite of AFB1, was employed as internal standard. Olive oil extract was analyzed by LC/ESI-MS/MS in positive ionization mode, with multireaction monitoring acquisition. Due to a signal suppression ranging between 4 and 23%, quantitation was performed by matrix-matched calibration curves. The regression line coefficients of determination were above 0.9991. Sample recoveries ranged from 92 to 107%, with relative standard deviations below 13% for spiking levels between 0.5 and 5 ng g(-1); method quantification limits ranged between 0.04 and 0.12 ng g(-1). The developed LC/ESI-MS/MS method, although not as sensitive as LC coupled to fluorescence detection, is rapid, selective, accurate and precise, thus it can be used as confirmatory assay. The MSPDE appears suitable for application to other oleaginous matrices and for multiresidue investigation.

摘要

本文提出了一种采用电喷雾电离的液相色谱 - 串联质谱法(LC/ESI-MS/MS)测定橄榄油中四种天然存在的黄曲霉毒素(AFs)B1、B2、G1和G2的方法。AFs通过基质固相分散法(MSPDE)从油样中提取,使用C18作为分散材料。未进行进一步的净化步骤,如去除脂质。黄曲霉毒素M1作为黄曲霉毒素B1的肝脏代谢产物,用作内标。橄榄油提取物通过LC/ESI-MS/MS在正离子模式下进行分析,采用多反应监测采集。由于信号抑制在4%至23%之间,通过基质匹配校准曲线进行定量。测定的回归线系数高于0.9991。样品回收率在92%至107%之间,对于0.5至5 ng g(-1)的加标水平,相对标准偏差低于13%;方法定量限在0.04至0.12 ng g(-1)之间。所开发的LC/ESI-MS/MS方法虽然不如与荧光检测联用的LC灵敏,但快速、选择性好、准确且精密,因此可作为确证分析方法。MSPDE似乎适用于其他含油基质以及多残留研究。

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