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开发一种使用高效液相色谱-串联质谱三重四极杆技术定量浓缩咖啡中木脂素的提取方法。

Development of an extraction method for the quantification of lignans in espresso coffee by using HPLC-MS/MS triple quadrupole.

作者信息

Angeloni Simone, Navarini Luciano, Sagratini Gianni, Torregiani Elisabetta, Vittori Sauro, Caprioli Giovanni

机构信息

School of Pharmacy, University of Camerino, via Sant' Agostino 1, 62032, Camerino, Italy.

illycaffè S.p.A., via Flavia 110, Trieste, I-34147, Italy.

出版信息

J Mass Spectrom. 2018 Sep;53(9):842-848. doi: 10.1002/jms.4251. Epub 2018 Jul 3.

Abstract

Lignans are polyphenolic compounds that are considered phytoestrogens for their plant origins, and they possess different biological activities. Three different extraction methods, ie, "dilute and shoot", acidic hydrolysis, and enzymatic digestion, have been compared for extracting lignans (secoisolariciresinol (SECO), matairesinol (MAT), and lariciresinol (LARI)) from espresso coffee (EC) by using high-performance liquid chromatography (HPLC) tandem mass spectrometry (MS/MS). The best recovery values (SECO: 97%, LARI: 98%, and MAT: 93%) were obtained by using enzymatic hydrolysis with Clara-Diastase at 10% (w/v), keeping the sample at 37°C for 3 hours. For this reason, this method has been chosen and then applied to quantify lignans in 9 different EC samples from 5 different geographical origins (Brazil, Colombia, El Salvador, Ethiopia, and India). Secoisolariciresinol and LARI were found in all EC samples from 27.9 to 52.0 μg L and from 5.3 to 27.8 μg L respectively, contrary to MAT that it was not possible to detect it in each type of coffee. This method confirms the high specificity and sensitivity of MS/MS system for detecting bioactives in complex matrix such as coffee.

摘要

木脂素是一类多酚化合物,因其源自植物而被视为植物雌激素,且具有不同的生物活性。已比较了三种不同的提取方法,即“稀释与喷射”法、酸性水解法和酶消化法,通过高效液相色谱(HPLC)串联质谱(MS/MS)从浓缩咖啡(EC)中提取木脂素(开环异落叶松脂素(SECO)、罗汉松脂素(MAT)和落叶松脂素(LARI))。使用10%(w/v)的克拉拉淀粉酶进行酶消化,将样品在37°C下保持3小时,可获得最佳回收率(SECO:97%,LARI:98%,MAT:93%)。因此,选择了该方法,然后将其应用于对来自5个不同地理来源(巴西、哥伦比亚、萨尔瓦多、埃塞俄比亚和印度)的9个不同浓缩咖啡样品中的木脂素进行定量。在所有浓缩咖啡样品中均检测到开环异落叶松脂素和落叶松脂素,含量分别为27.9至52.0μg/L和5.3至27.8μg/L,而罗汉松脂素在每种咖啡中均未检测到。该方法证实了MS/MS系统在检测咖啡等复杂基质中的生物活性成分方面具有高特异性和高灵敏度。

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