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[摘要]
本研究建立了一种高效液相色谱法同时测定油茶籽油中γ-生育酚、β-谷甾醇和角鲨烯。油茶籽油样品经过皂化、萃取、浓缩,将油茶籽油中的皂化物类成分除去,富集其中的不皂化物类成分,并通过HPLC进行分析检测,按外标法测定其含量。HPLC色谱条件:色谱柱Hypersil ODS C18(250 mm×4.6 mm,5 μm);流动相为100%甲醇,等度洗脱;流速0.7 mL/min;柱温30 ℃;检测波长:205 nm。结果表明γ-生育酚、β-谷甾醇和角鲨烯分别在0.01~0.40 μg(R2=0.9999)、0.44~10.94 μg(R2=1)、0.01~0.55 μg(R2=0.9990)范围内呈较好的线性关系,相关系数均接近1。平均加样回收率分别为97.1322%(RSD=1.28%)、100.2346%(RSD=1.54%)、98.0859%(RSD=1.58%),相对标准偏差均小于3%。结论:该方法前处理简单易行,操作简便,灵敏度高,重现性和准确性好,可用于油茶籽油中γ-生育酚、β-谷甾醇和角鲨烯的含量测定和油茶籽油质量控制。
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[Abstract]
A high performance liquid chromatography (HPLC) method was developed for the simultaneous determination of γ-antisterility vitamin, β-sitosterol, squalene in camellia oil. The camellia oil samples were saponified, extracted and concentrated to remove the saponifiable substance in camellia oil, and the unsaponified material component was enriched. The content of the saponification products were determined by HPLC and analyzed by external standard method. Hypersil ODS C18 (250 mm × 4.6 mm, 5 μm) chromatography column was used for the determination under the conditions of mobile phase methanol (volume ratio 100%) and detection wavelength 205 nm. The column temperature was 30 oC and the flow rate was 0.7 mL/min. The results showed that correlation coefficients were all close to 1 for γ-antisterility vitamin, β-sitosterol and squalene in the range of 0.01~0.40 μg (R2=0.9999), 0.44~10.94 μg (R2=1) and 0.01~0.55 μg (R2=0.9990), respectively. reThe average recovery was 97.1322% (RSD=1.28%), 100.2346% (RSD=1.54%), 98.0859% (RSD=1.58%), and the relative standard deviations were all less than 3%. The proposed method had the advantages of simple pretreament, easy operation, high sensitivity, good accuracy and reproducibility, and could be used for the determination of γ-antisterility vitamin, β-sitosterol, squalene in camellia oil and the evaluation for the quality of camellia oil.
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