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一种验证的 LC-MS/MS 方法,用于定量测定 Sarconi 豆(菜豆属)中的左旋多巴。

A validated LC-MS/MS method for quantitative determination of L-dopa in Fagioli di Sarconi beans (Phaseolus vulgaris L.).

机构信息

Department of Sciences, University of Basilicata, Potenza, Italy.

Department of Pharmacy, University of the Study of Salerno, Fisciano, Italy.

出版信息

J Mass Spectrom. 2023 Oct;58(10):e4952. doi: 10.1002/jms.4952. Epub 2023 Jul 3.

DOI:10.1002/jms.4952
PMID:37401097
Abstract

An analytical method based on ultrasound assisted extraction (UAE) and liquid chromatography coupled to electrospray tandem mass spectrometry (LC-ESI/MS/MS) was validated and applied for determining L-dopa in four ecotypes of Fagioli di Sarconi beans (Phaseolus vulgaris L.), marked with the European label PGI (Protected Geographical Indication). The selectivity of the proposed method was ensured by the specific fragmentation of the analyte. Simple isocratic chromatographic conditions and mass spectrometric detection in multiple reaction monitoring (MRM) acquisition mode were used for sensitive quantification. The LC-ESI/MS/MS method was validated within a linear range of 0.001-5.000 μg/mL. Values of 0.4 and 1.1 ng/mL were obtained for the limits of detection and quantification, respectively. The repeatability, inter-day precision, and recovery values ranges were 0.6%-4.5%, 5.4%-9.9%, and 83%-93%, respectively. Fresh and dried beans, as well as pods, cultivated exclusively with organic methods avoiding any synthetic fertilizers and pesticides were analyzed showing an L-dopa content ranging from 0.020 ± 0.005 to 2.34 ± 0.05 μg/g dry weight.

摘要

基于超声辅助提取 (UAE) 和液相色谱-电喷雾串联质谱 (LC-ESI/MS/MS) 的分析方法得到了验证,并应用于测定四个生态型的 Sarconi 豆(Phaseolus vulgaris L.)中的左旋多巴(L-dopa),这些豆被贴上了欧洲 PGI(受保护地理标志)标签。该方法的选择性通过分析物的特定碎片得到保证。简单的等度色谱条件和在多反应监测 (MRM) 采集模式下的质谱检测用于进行灵敏的定量分析。LC-ESI/MS/MS 方法在 0.001-5.000 μg/mL 的线性范围内进行了验证。检测限和定量限的值分别为 0.4 和 1.1 ng/mL。重复性、日间精密度和回收率的范围分别为 0.6%-4.5%、5.4%-9.9%和 83%-93%。采用有机方法(避免使用任何合成肥料和农药)专门种植的新鲜和干燥的豆以及豆荚进行了分析,其左旋多巴含量范围为 0.020±0.005 至 2.34±0.05 μg/g 干重。

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