Optimization and validation of an HPLC-HRMS method through semipreparative HPLC system for determining phytosterol oxidation products during refining processing and storage of vegetable oils

IF 1.9 4区 农林科学 Q3 CHEMISTRY, APPLIED Journal of the American Oil Chemists Society Pub Date : 2024-02-26 DOI:10.1002/aocs.12826
Raffaele Calaminici, Nicolò Ivan Salgarella, Vladimiro Cardenia, Emanuele Forte
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Abstract

A semi-preparative liquid chromatographic system (LC-Prep) has been used to isolate and collect the main oxidation products generated from β-sitosterol, campesterol, and stigmasterol, which represent the main sterols detected in vegetable oils. In less than 50 min, 15 different phytosterol oxidation products (POPs) were separated with a satisfactory resolution (R >1) and collected. From each pure phytosterol standard the 5,6α-epoxy (α-E), 5,6β-epoxy (β-E), 7-keto (7-K), 7α-hydroxy (7α-H), and 7β-hydroxy (7β-H) isomers were obtained. The purity of POPs was >90%. Then, the obtained pure POPs were used to validate an HPLC-Orbitrap-HRMS analytical method. The LOD and LOQ determined in medium chain triacylglycerols were >0.012 and >0.039 ng/mL, respectively; whereas the recoveries ranged between 82% and 98%. The suitability of the analytical method was evaluated on palm oil (PO), palm olein (POL), and high oleic sunflower oil (HOSO) during the whole refining processing (crude oil, neutralization and degumming, bleaching and deodorization) and under storage conditions (45°C, 16 days). In the refining steps, the total POPs content significantly increased (p < 0.05) by 29%, 20%, and 13% in PO, POL, and HOSO, respectively. The highest amount was found in HOSO (15.046 mg/kg), followed by POL (1.067 mg/kg) and PO (0.538 mg/kg). Under storage conditions, the content of POPs did not significantly (p > 0.05) change and was lower than 8.965 mg/kg. The developed semi-preparative liquid chromatographic system coupled to the LC-Orbitrap-HRMS method demonstrated to be a useful and valid tool for a robust, precise, accurate, and sensitive determination of POPs in refined and stored vegetable oils.

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通过半制备高效液相色谱系统优化和验证测定植物油精炼加工和储存过程中植物甾醇氧化产物的高效液相色谱-HRMS 方法
采用半制备液相色谱系统(LC-Prep)分离并收集了植物油中检测到的主要甾醇--β-谷甾醇、坎贝酯醇和豆固醇产生的主要氧化产物。在不到 50 分钟的时间内,就分离并收集了 15 种不同的植物甾醇氧化产物(POPs),其分辨率令人满意(R >1)。从每种纯植物甾醇标准物质中都能得到 5,6α-epoxy (α-E), 5,6β-epoxy (β-E), 7-keto (7-K), 7α-hydroxy (7α-H) 和 7β-hydroxy (7β-H) 异构体。持久性有机污染物的纯度为 90%。然后,用获得的纯持久性有机污染物验证了 HPLC-Orbitrap-HRMS 分析方法。在中链三酰甘油中测定的LOD和LOQ分别为0.012和0.039 ng/mL,回收率为82%至98%。对棕榈油(PO)、棕榈油精(POL)和高油酸葵花籽油(HOSO)在整个精炼加工过程(毛油、中和脱胶、漂白和除臭)和储存条件(45°C,16 天)下的分析方法的适用性进行了评估。在精炼步骤中,PO、POL 和 HOSO 中的持久性有机污染物总含量分别显著增加了 29%、20% 和 13%(p < 0.05)。含量最高的是 HOSO(15.046 毫克/千克),其次是 POL(1.067 毫克/千克)和 PO(0.538 毫克/千克)。在贮存条件下,持久性有机污染物的含量变化不大(p > 0.05),低于 8.965 毫克/千克。所开发的半制备液相色谱系统与 LC-Orbitrap-HRMS 方法相结合,证明是一种有效的工具,可用于稳健、精确、准确、灵敏地测定精炼和储藏植物油中的持久性有机污染物。
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来源期刊
CiteScore
4.10
自引率
5.00%
发文量
95
审稿时长
2.4 months
期刊介绍: The Journal of the American Oil Chemists’ Society (JAOCS) is an international peer-reviewed journal that publishes significant original scientific research and technological advances on fats, oils, oilseed proteins, and related materials through original research articles, invited reviews, short communications, and letters to the editor. We seek to publish reports that will significantly advance scientific understanding through hypothesis driven research, innovations, and important new information pertaining to analysis, properties, processing, products, and applications of these food and industrial resources. Breakthroughs in food science and technology, biotechnology (including genomics, biomechanisms, biocatalysis and bioprocessing), and industrial products and applications are particularly appropriate. JAOCS also considers reports on the lipid composition of new, unique, and traditional sources of lipids that definitively address a research hypothesis and advances scientific understanding. However, the genus and species of the source must be verified by appropriate means of classification. In addition, the GPS location of the harvested materials and seed or vegetative samples should be deposited in an accredited germplasm repository. Compositional data suitable for Original Research Articles must embody replicated estimate of tissue constituents, such as oil, protein, carbohydrate, fatty acid, phospholipid, tocopherol, sterol, and carotenoid compositions. Other components unique to the specific plant or animal source may be reported. Furthermore, lipid composition papers should incorporate elements of year­to­year, environmental, and/ or cultivar variations through use of appropriate statistical analyses.
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Issue Information Issue Information Microfluidization outperforms homogenization: Optimizing stability and bioaccessibility in krill oil emulsions Issue Information JAOCS special issue on advancement in plant protein-based emulsions
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