| 周晓娇1,2， 谢枫才1,3， 陈敏嫣1,2,等.分子蒸馏联用制备液相色谱法制备 高纯度DHA乙酯及抗氧化性能研究[J].中国油脂,2021,46(5):.[ZHOU Xiaojiao1,2, XIE Fengcai1,3, CHEN Minyan1,2,ets.Preparation of high purity DHA ethyl ester by molecular distillation and preparative liquid chromatography[J].China Oils and Fats,2021,46(5):.] |
| 分子蒸馏联用制备液相色谱法制备 高纯度DHA乙酯及抗氧化性能研究 |
| Preparation of high purity DHA ethyl ester by molecular distillation and preparative liquid chromatography |
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| DOI： |
| 中文关键词: DHA乙酯 高纯度 分子蒸馏 制备液相色谱 |
| 英文关键词:DHA-EE high purity molecular distillation preparative liquid chromatograph |
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| 中文摘要: |
| 探讨藻油中二十二碳六烯酸（DHA）分离纯化工艺，通过改进工艺条件获得高纯度DHA乙酯（DHA-EE）。以乙酯化藻油为原料，采用分子蒸馏联用制备液相色谱法制备高纯度DHA-EE，通过单因素实验优化工艺条件。结果表明：最优分子蒸馏条件为蒸发温度105?℃、内冷凝温度55?℃、外冷凝温度30?℃、物料温度30?℃、刮膜速率160 r/min、真空度1 Pa、进料速度1 g/min，在此条件下DHA-EE纯度为72.1%，回收率为71.6%；最优制备液相色谱条件为采用YMC-PACK ODS-A制备柱（5 μm，21.1 mm×250 mm）、流动相甲醇-水（体积比95∶?5）、流速20 mL/min、上样量0.2 g、检测波长204 nm，在此条件下 DHA-EE纯度达到96%以上，平均回收率为79.66%。 |
| 英文摘要: |
| The separation and purification process of decosahexaenoic acid (DHA) in algae oil were discussed, and high purity DHA ethyl ester (DHA-EE) was obtained by improving the process conditions. Using ethylated algae oil as the raw material, high purity DHA-EE was prepared by molecular distillation and preparative liquid chromatography, and the process conditions were optimized by single factor experiment. The results showed that the optimal molecular distillation conditions were obtained as follows: evaporation temperature 105?℃, internal condensation temperature 55?℃, external condensation temperature 30?℃, material temperature 30?℃, rotation speed 160 r/min, vacuum degree 1 Pa, and feed rate 1 g/min. Under these conditions, the purity of DHA-EE was 72.1%, and the recovery rate was 716%. The optimal preparative liquid chromatography conditions were obtained as follows: using YMC-PACK ODS-A preparation column(5 μm,21.1 mm×250 mm), with methanol-water (volume ratio 95∶?5) as mobile phase, flow rate 20 mL/min, loading amount 0.2 g and detection wavelength 204 nm. Under these conditions, the DHA-EE purity reached more than 96%, and the average recovery rate was 79.66%. |
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