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| 初榨葡萄籽毛油中维生素E、植物甾醇及角鲨烯的快速同步检测 |
| Rapid simultaneous determination of vitamin E, phytosterol and squalene in virgin crude grape seed oil |
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| DOI： |
| 中文关键词: 初榨葡萄籽毛油 植物甾醇 谷甾烷醇 角鲨烯 生育三烯酚 生育酚 |
| 英文关键词:virgin crude grape seed oil phytos terol stanol squalene tocotrienol tocopherol |
| 基金项目: |
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| 中文摘要: |
| 建立一种高准确度、快速的HPLC方法测定初榨葡萄籽毛油中维生素E、植物甾醇（菜油甾醇、豆甾醇、 β-谷甾醇、谷甾烷醇）及角鲨烯的含量。样品经高温皂化，以无水乙醚为提取剂提取，纯化后采用HPLC检测。流动相采用A相甲醇-乙腈-叔丁基甲醚（体积比85.5∶?8∶?6.5），B相超纯水-冰醋酸（体积比99∶?1），梯度洗脱，进样量20 μL，流速1.0 mL/min，维生素E与3种常见植物甾醇、角鲨烯检测波长分别为292 nm与210 nm，柱温25?℃，谷甾烷醇采用ELSD检测，运行时间25 min。结果表明：11种目标物的质量浓度均与峰面积有较好的线性关系，R2均大于0.999，检出限为0.10~5.00 μg/mL，定量限为0.17~6.25 μg/mL；样品中维生素E总含量为357.09~655.06 mg/kg，植物甾醇总含量为1 220.11~3 178.76 mg/kg，角鲨烯含量为24.21~67.98 mg/kg。该方法测定相对偏差较小，结果准确，可以成批次测定初榨葡萄籽毛油。 |
| 英文摘要: |
| An accurate and fast method was established to detect vitamin E, phytosterol(campesterol,stigmasterol,β-sitosterol, stanol) and squalene content in virgin crude grape seed oil by HPLC. Sample was saponificated at high temperature, then extracted by absolute ethyl ether, purified and detected by HPLC. HPLC conditions were obtained as follows: mobile phase A methanol-acetonitrile-TBME(volume ratio 85.5∶?8∶?6.5),mobile phase B water-acetic acid(volume ratio 99∶?1), injection volume 20 μL, detection wavelength 292 nm for vitamin E, 210 nm for campesterol, stigmasterol and β-sitosterol and squalene, column temperature 25 ?℃, ELSD for stanol and operation time 25 min. The results showed that the mass concentrations and peark areas of eleven target objects had a good linear relationship (R2＞0.999). The detection limit was 0.10-5.00 μg/mL, and the quantification limit was 0.17-6.25 μg/mL. The vitamin E content in the sample was 357.09-655.06 mg/kg, the phytosterol content was 1 220.11-3 178.76 mg/kg, and the squalene content was 24.21-67.98 mg/kg. The method had the items of low RSD and accurate result, and could be used to detect virgin crude grape seed oil in batch. |
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