Separation and determination of diversiform phytosterols in food materials using supercritical carbon dioxide extraction and ultraperformance liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry |
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Authors: | Lu Baiyi Zhang Ying Wu Xiaoqin Shi Jiayi |
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Affiliation: | Department of Food Science and Nutrition, College of Biosystems Engineering and Food Science, Zhejiang University, Hangzhou 310029, Zhejiang Province, PR China |
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Abstract: | This paper presents at first time that the ultra-performance™ liquid chromatographic atmospheric pressure chemical ionization mass spectrometer (UPLC-APCI-MS) was used as an efficient method for the identification and quantification of diversiform phytosterols in food materials. The sample preparation consisted of extraction by supercritical carbon dioxide fluid extraction (SCE) and saponification by refluxing with ethanolic KOH, and then the non-saponificable fraction was extracted with petroleum ether. This fraction was subjected to solid phase extraction (SPE) on silica gel cartridge and then the sterols were eluted with hexane-ethyl acetate. Sterols were separated on an Acquity UPLC™ BEH C18 column (100 mm × 1.0 mm, 1.7 μm particle size) with a gradient of methanol/water (1% acetonitrile) at a flow of 0.1 mL min−1. The determination was performed in selective ion monitoring mode. The quality parameter of the developed method was established using 6-ketocholestanol as internal standard. Limits of quantification (LOQ) were 0.1754, 0.0341, 0.0500, 0.0205, 0.0225, 0.3674, 0.0241, 0.0272, 0.0076 μg L−1 and 0.1525 μg mL−1 for 6-ketocholestanol, desmosterol, ergosterol, cholesterol, lanosterol, cholestanol, campesterol, stigmasterol, β-sitosterol, and stigmastanol, respectively. The intra- and inter-day determination precision for the 10 phytosterols were less than 5 and 6% in relative standard deviations, and their recoveries were located in the range of 94-107%. The developed approach has been applied successfully for efficient determination of diversiform phytosterols in food materials, including corn, sesame, oat and peanut. |
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Keywords: | UPLC-MS, ultra-performance&trade liquid chromatographic-mass spectrometer APCI, atmospheric pressure chemical ionization SIM, selective ion monitoring LOD, limits of detection LOQ, limits of quantification SCE, supercritical carbon dioxide extraction SPE, solid phase extraction |
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