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采用高效液相色谱-串联质谱法定量测定猪血浆中的展青霉素、恩镰菌素 A、A1、B 和 B1 等镰刀菌真菌毒素。

Quantitative determination of the Fusarium mycotoxins beauvericin, enniatin A, A1, B and B1 in pig plasma using high performance liquid chromatography-tandem mass spectrometry.

机构信息

Department of Pharmacology, Toxicology and Biochemistry, Faculty of Veterinary Medicine, Ghent University, Salisburylaan 133, 9820 Merelbeke, Belgium.

出版信息

Talanta. 2013 Mar 15;106:212-9. doi: 10.1016/j.talanta.2012.11.068. Epub 2012 Dec 19.

Abstract

A sensitive and reliable method was developed for the identification and quantification of beauvericin, enniatin A, A1, B and B1 in pig plasma using liquid chromatography combined with heated electrospray ionization tandem mass spectrometry. Sample clean-up consisted of a deproteinization step using acetonitrile, followed by evaporation of the supernatant and resuspension of the dry residue in acetonitrile/water (80/20, v/v). The method was in-house validated: matrix-matched calibration graphs were prepared for all compounds and correlation and goodness-of-fit coefficients ranged between 0.9980 and 0.9995 and between 5.2% and 11.3%, respectively. The within- and between-run precision and accuracy were evaluated and the results fell within the ranges specified. The limits of quantification were 0.1 ng/mL for enniatin A and A1 and 0.2 ng/mL for beauvericin, enniatin B and B1, whereas limits of detection were ≤ 10 pg/mL for all analytes. The method has been applied for the analysis of real plasma samples from one pig that received an oral bolus (0.05 mg/kg BW) of the investigated mycotoxins. At the applied dosage, the results indicated the suitability of the method for use in toxicokinetic studies with enniatins.

摘要

建立了一种灵敏、可靠的方法,用于猪血浆中 beauvericin、enniatin A、A1、B 和 B1 的鉴定和定量,该方法采用液相色谱-加热电喷雾串联质谱法。样品净化包括使用乙腈进行蛋白沉淀步骤,然后蒸发上清液并将干燥残渣重新悬浮于乙腈/水(80/20,v/v)中。该方法是内部验证的:为所有化合物制备了基质匹配校准曲线,相关系数和拟合优度系数在 0.9980 到 0.9995 之间,分别在 5.2%到 11.3%之间。评估了批内和批间精密度和准确度,结果在规定范围内。enniatin A 和 A1 的定量限为 0.1 ng/mL,beauvericin、enniatin B 和 B1 的定量限为 0.2 ng/mL,而所有分析物的检测限均≤10 pg/mL。该方法已应用于分析一只猪口服(0.05 mg/kg BW)研究真菌毒素后的实际血浆样品。在应用剂量下,结果表明该方法适用于 enniatins 的毒代动力学研究。

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