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通过苯基-己基柱制备高效液相色谱法从亚麻籽油中快速提取 12 种环丝氨酸(linusorbs)。

A practical and fast isolation of 12 cyclolinopeptides (linusorbs) from flaxseed oil via preparative HPLC with phenyl-hexyl column.

机构信息

Guangdong Saskatchewan Oilseed Joint Laboratory, Department of Food Science and Engineering, Jinan University, Guangzhou 510632, China.

Guangdong Saskatchewan Oilseed Joint Laboratory, Department of Food Science and Engineering, Jinan University, Guangzhou 510632, China; Department of Plant Sciences, University of Saskatchewan, 51 Campus Dr., Saskatoon, SK, S7N 5A8, Canada.

出版信息

Food Chem. 2021 Jul 30;351:129318. doi: 10.1016/j.foodchem.2021.129318. Epub 2021 Feb 18.

DOI:10.1016/j.foodchem.2021.129318
PMID:33647690
Abstract

Linusorbs, known as cyclolinopeptides, are a group of cyclic hydrophobic peptides derived from flaxseed oil with various health benefits. However, the current research efforts on both the biological activities and antioxidant capacities of linusorbs are limited because of existing issues with their purification and characterization. A practical method based on preparative HPLC for isolating 12 linusorbs simultaneously was developed and factors such as the solvent selection, gradient elution program, flow rate, loaded mass, and loading concentration, were optimized. The optimum conditions were an initial acetonitrile (ACN) to water ratio of 40%, final ACN ratio of 80%, eluting time of 21 min, a flow rate of 16 mL/min, sample load of 12.5 mg, and concentration of 80 mg/mL (in methanol). The 12 linusorbs obtained were verified using off-line MS/MS, recording purities of above 95.5%. The method could serve as a practical and fast isolation method enabling further investigation of minor linusorbs.

摘要

亚麻小肽,又称环松萝肽,是一类从亚麻籽油中衍生出的具有多种健康益处的环状疏水性肽。然而,由于其纯化和表征方面存在的问题,目前对亚麻小肽的生物活性和抗氧化能力的研究工作十分有限。本研究建立了一种基于制备高效液相色谱法(HPLC)同时分离 12 种亚麻小肽的实用方法,并对溶剂选择、梯度洗脱程序、流速、上样量和上样浓度等因素进行了优化。优化后的条件为:初始乙腈(ACN)与水的比例为 40%,最终 ACN 比例为 80%,洗脱时间为 21 分钟,流速为 16 mL/min,样品上样量为 12.5mg,浓度为 80mg/mL(在甲醇中)。使用离线 MS/MS 对得到的 12 种亚麻小肽进行验证,纯度均高于 95.5%。该方法可作为一种实用且快速的分离方法,可进一步研究含量较低的亚麻小肽。

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