【作者】 匡勇娇；

【导师】 王永宁；

【作者基本信息】 青海师范大学 ， 无机化学， 2010， 硕士

【摘要】 本课题以青藏高原油菜蜂花粉为原料，采用生物酶法破壁，然后较为系统地研究了破壁和未破壁油菜蜂花粉油的提取、理化性质的测定和脂肪酸分析，为开发和利用青藏高原丰富的油菜蜂花粉资源提供了理论依据和优化的工艺方法。研究结果如下：1.超临界CO₂萃取油菜蜂花粉油的工艺切实可行，其最佳工艺：萃取压力为20MPa，萃取温度为35℃，CO₂流速为15L/h，一级分离的压力为8MPa，一级分离的温度为55℃，花粉粒度为20～40目，萃取时间2～3h。最佳条件下，破壁油菜蜂花粉油的萃取率为9.69%，未破壁油菜蜂花粉油的萃取率为9.25%。2.石油醚冷浸提取油菜蜂花粉油的最佳条件是浸提时间为36h，固液比为1：15g/mL，花粉粒度为40～60目。在最佳条件下，破壁油菜蜂花粉油得率为8.73%，未破壁花粉油得率为7.81%。3.经测定并比较超临界CO₂萃取法和石油醚冷浸提取法萃取的破壁和未破壁油菜蜂花粉油的理化性质，超临界CO₂萃取法是较为理想的提取方法。超临界CO₂萃取法制得的破壁油菜粉花粉油水分及挥发物含量为0.038%、折光指数(n²⁵)为1.4933、酸价为10.49mgKOH/g、皂化价为148.40、过氧化价为9.6meq/kg、碘价为149.57、由燃烧热测定方法测得的热值为41.75KJ/g；超临界CO₂萃取法制得的未破壁油菜粉花粉油水分及挥发物含量为0.039%、折光指数(n²⁵)为1.4916、酸价为13.31mgKOH/g、皂化价为101.61、过氧化价为9.4meq/kg、碘价为147.23、由燃烧热测定方法测得的热值为42.37KJ/g。4.确定了最佳色谱条件：柱温：采用程序升温条件为110℃（3min）10℃/min240℃（20min）；检测器的温度250℃；分流进样模式；气化室温度250℃；H2 :Air流量比50：500mL/min。简易碱式甲酯化方法的较佳的反应条件为：正己烷-乙醚（1：2）作为萃取剂，0.5mol/L的甲醇钠甲醇溶液作为衍生催化剂，反应时间为10min。在最佳的色谱分析条件和甲酯化条件建立后，对用不同方法提取的破壁和未破壁油菜蜂花粉油中的脂肪酸进行了定性和定量分析，并且对其中的脂肪酸组成进行了比较。更多还原

【Abstract】 The study using Qinghai-Tibet Plateau rape bee pollen as raw material and the biological enzymatic wall-broken method, focused on extraction of the wall-broken and wall-unbroken Rape bee pollen oil, analysis of its physical-chemical properties and fatty acid composition. It supplied a theoretic basis and optimum processing technics for empoldering and utilizing the rich resources of rape bee pollen of the Qinghai-Tibet Plateau.The results of the study were as followings.1. The process of supercritical carbon dioxide extraction of rape bee pollen oil was practicable, its optimum condition of extraction were as follows: extraction pressure and separation I pressure were 20MPa and 8MPa respectively. Extraction temperature and separation I temperature was 35℃and 55℃respectively. CO₂ flow rate was 15L/h. The grain size of pollen was 20～40 mesh.Extraction time was 2～3h. The extraction rate of wall-broken and wall-unbroken rape bee pollen oil was 9.69% and 9.25% in the optimum condition, respectively.2. The optimum cold soak extraction conditions of fatty Acids in rape bee pollen of the Qinghai-Tibet Plateau with petroleum ether as solvent: extraction time was 36 hours. The ratio of the pollen weight and solvent volume was 1:15（g/mL）. The grain size of pollen was greater than 40 mesh. The yield ratios of wall-broken and wall-unbroken rape bee pollen oil were 8.73% and 7.81% in the optimum condition, respectively.3. It was testified by determining the physical-chemical properties of wall-broken and wall-unbroken rape bee pollen oil and then comparing them that supercritical CO₂ extraction was better than petroleum ether cold soak extraction. The content of moisture and volatile, refractive index (n²⁵), acid value, saponification value, peroxide value, iodine value, the burning heat value of wall-broken rape bee pollen oil extracted by Supercritical CO₂ extraction were 0.038%, 1.4933, 10.49mgKOH/g, 148.40, 9.6meq/kg, 149.57, 41.75KJ/g, respectively. The ones of wall-unbroken rape bee pollen oil extracted by Supercritical CO₂ extraction were 0.039%, 1.4916, 13.31mg KOH/g, 101.61, 9.4 meq/kg, 147.23, 42.37KJ/g, respectively.4. The optimum chromatographic conditions were found: oven tempera -ture: temperature-programmed conditions was 110℃（3min）10℃/ min240℃（20min）; detector temperature: 250℃; injector temperature: 250℃; split injection; flow ratio of H2:Air: 50:500mL/min. The better reaction conditions of the simplified method of alkaline methylesterefication were as follows: n-hexane-ether （1:2） as extractant, 0.5mol/L sodium methoxide in methanol solution as derived catalyst, reaction time for 10min. The wall-broken and wall-unbroken rape bee pollen oils which were extracted by different methods were analyzed qualitatively and quantitatively and the fatty acids compositions were compared in the optimum chromatographic and methyl -esterefication conditions.更多还原