松针聚戊烯醇的制备及性质研究
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摘要
本课题以雪松松针为原料,对松针聚戊烯醇及其乙酸酯的提取、水解、纯化工艺、结构、稳定性及抗氧化性进行了较为系统的研究与分析,为松针聚戊烯醇的开发、应用提供理论参考和科学依据。主要研究结论如下:
松针聚戊烯醇及其乙酸酯在不同月份含量不同,9-11月份含量最高。通过单因素和响应面法分析,获得松针聚戊烯醇及其乙酸酯的最佳提取工艺为:以石油醚为溶剂,采用超声波法,料液比为1:8.5g/mL,超声功率为90W,超声时间为62min,超声温度为42℃。通过薄层色谱检测,获得聚戊烯醇乙酸酯的水解条件为:5%NaOH-甲醇溶液,30℃下热回流磁力搅拌2.5h。松针粗提聚戊烯醇浸膏脱蜡的条件为:在0℃左右采用1:10g/mL丙酮:乙酸乙酯(9:1)进行脱蜡。
采用吸附柱色谱对松针聚戊烯醇进行纯化,薄层色谱检测得纯化的工艺参数为:100-200目硅胶,先采用石油醚洗脱,再采用石油醚:乙酸乙酯(19:1)洗脱,洗脱流速≤1mL/min。薄层色谱检测,收集聚戊烯醇组分,减压浓缩,真空干燥制得聚戊烯醇样品。通过紫外、红外对松针样品进行结构鉴定,高效液相-质谱检测出5个单体,其异戊烯基单元数为23、21、20、18、15。
温度对松针聚戊烯醇的稳定性影响较显著:当温度≤30℃时,聚戊烯醇的吸光值变化较小,稳定性较好,因此,聚戊烯醇在≤30℃下保存较好;光照对松针聚戊烯醇的稳定性有一定影响,最好避光保存;松针聚戊烯醇对酸碱度较敏感:强酸、强碱对聚戊烯醇的稳定性影响较显著,在中性、弱酸或弱碱状态下聚戊烯醇较稳定;金属离子对松针聚戊烯醇的影响:Ca~(2+)、Cu~(2+)、Al~(3+)、Zn~(2+)、K~+、Mg~(2+)对聚戊烯醇的稳定性影响不大;Fe~(3+)、Fe~(2+)、Ag~+随着浓度的增大对聚戊烯醇的稳定性影响较显著。
松针聚戊烯醇属于类脂化合物,其酸价、碘价、皂化价依次为3.89 mg KOH/g、2.65 mg KOH/g、2.06 mg KOH/g;采用邻苯三酚自氧化法进行测定,对邻苯三酚自氧化的抑制率为23.1%。
The task’s material is from pine needle of cedar,making a systematic study and analysis about extraction,hydrolysis,purification,stability and so on of pine needle polyprenols and acetic ester,providing theoretical reference and scientific basis.The main conclusions are as follows:
The content of pine needle polyprenols and acetic ester is different on different months,the content from September to November is higher.The beauty extracting technology by single factor and response surface method is:petroleum is solvent,ultrasonic as extracting method,ratio of solid to liquid is 8.5g/mL,ultrasonic power is 90W,ultrasonic time is 62min,ultrasonic temperature is 42℃.The hydrolysis condition of pine needle polyprenol acetic ester is:5%NaOH-CH_3OH solution,hot reflux magnetic force stirring 2.5h on 30℃. The optimization condition of dewaxing on the extractum of pine needle polyprenols is:adopting acetone 1:10g/mL:acetic ether(9:1)on 0℃.
The purification of pine needle polyprenols is by the method of adsorption chromatograph,the technological parameter is:100-200 silica gel,firstly eluting by petroleum ether,secondly eluting by petroleum ether:acetic ether(19:1),the flow velocity is under 1 mL/min.Thin layer chromatography detection,colleting polyprenols,reduced pressure distillation,vacuum and freeze drying for the sample of polyprenols.The pine needle polyprenols have five monocases,whose M of isopentene group is twenty three,twenty one ,twenty,eighteen,fifteen.
The effect of temperature on pine needle polyprenols is notability:when temperature is under 30℃,the change of pine needle polyprenols’absorbance,the stability is better,therefore,the conservation of pine needle polyprenols should be under 30℃;the illumination make an effect on pine needle polyprenols stability,which should be conserved on darkness;the pine needle polyprenols is sensitivity on different pH : strong acid and strong alkali is notability to pine needle polyrenols,pine needle polyprenols is stability on neutral or weak acid and alkali.The effect of metal ions on pine needle polyprenols:the effect of pine needle polyprenols stability is little by Ca~(2+),Cu~(2+),Al~(3+),Zn~(2+),K~+,Mg~(2+);the effect of pine needle polyprenols stability is much notability by Fe~(3+),Fe~(2+),Ag~+.
The polyprenols is belong to lipoids,whose acid value,iodine value and saponification value of pine needle polyprenols is 3.89 mg KOH/g,2.65 mg KOH/g,2.06 mg KOH/g;The clearance of pine needle polyprenols is up to 23.1% by the method of pyrogallol auto-oxidation.
松针聚戊烯醇及其乙酸酯在不同月份含量不同,9-11月份含量最高。通过单因素和响应面法分析,获得松针聚戊烯醇及其乙酸酯的最佳提取工艺为:以石油醚为溶剂,采用超声波法,料液比为1:8.5g/mL,超声功率为90W,超声时间为62min,超声温度为42℃。通过薄层色谱检测,获得聚戊烯醇乙酸酯的水解条件为:5%NaOH-甲醇溶液,30℃下热回流磁力搅拌2.5h。松针粗提聚戊烯醇浸膏脱蜡的条件为:在0℃左右采用1:10g/mL丙酮:乙酸乙酯(9:1)进行脱蜡。
采用吸附柱色谱对松针聚戊烯醇进行纯化,薄层色谱检测得纯化的工艺参数为:100-200目硅胶,先采用石油醚洗脱,再采用石油醚:乙酸乙酯(19:1)洗脱,洗脱流速≤1mL/min。薄层色谱检测,收集聚戊烯醇组分,减压浓缩,真空干燥制得聚戊烯醇样品。通过紫外、红外对松针样品进行结构鉴定,高效液相-质谱检测出5个单体,其异戊烯基单元数为23、21、20、18、15。
温度对松针聚戊烯醇的稳定性影响较显著:当温度≤30℃时,聚戊烯醇的吸光值变化较小,稳定性较好,因此,聚戊烯醇在≤30℃下保存较好;光照对松针聚戊烯醇的稳定性有一定影响,最好避光保存;松针聚戊烯醇对酸碱度较敏感:强酸、强碱对聚戊烯醇的稳定性影响较显著,在中性、弱酸或弱碱状态下聚戊烯醇较稳定;金属离子对松针聚戊烯醇的影响:Ca~(2+)、Cu~(2+)、Al~(3+)、Zn~(2+)、K~+、Mg~(2+)对聚戊烯醇的稳定性影响不大;Fe~(3+)、Fe~(2+)、Ag~+随着浓度的增大对聚戊烯醇的稳定性影响较显著。
松针聚戊烯醇属于类脂化合物,其酸价、碘价、皂化价依次为3.89 mg KOH/g、2.65 mg KOH/g、2.06 mg KOH/g;采用邻苯三酚自氧化法进行测定,对邻苯三酚自氧化的抑制率为23.1%。
The task’s material is from pine needle of cedar,making a systematic study and analysis about extraction,hydrolysis,purification,stability and so on of pine needle polyprenols and acetic ester,providing theoretical reference and scientific basis.The main conclusions are as follows:
The content of pine needle polyprenols and acetic ester is different on different months,the content from September to November is higher.The beauty extracting technology by single factor and response surface method is:petroleum is solvent,ultrasonic as extracting method,ratio of solid to liquid is 8.5g/mL,ultrasonic power is 90W,ultrasonic time is 62min,ultrasonic temperature is 42℃.The hydrolysis condition of pine needle polyprenol acetic ester is:5%NaOH-CH_3OH solution,hot reflux magnetic force stirring 2.5h on 30℃. The optimization condition of dewaxing on the extractum of pine needle polyprenols is:adopting acetone 1:10g/mL:acetic ether(9:1)on 0℃.
The purification of pine needle polyprenols is by the method of adsorption chromatograph,the technological parameter is:100-200 silica gel,firstly eluting by petroleum ether,secondly eluting by petroleum ether:acetic ether(19:1),the flow velocity is under 1 mL/min.Thin layer chromatography detection,colleting polyprenols,reduced pressure distillation,vacuum and freeze drying for the sample of polyprenols.The pine needle polyprenols have five monocases,whose M of isopentene group is twenty three,twenty one ,twenty,eighteen,fifteen.
The effect of temperature on pine needle polyprenols is notability:when temperature is under 30℃,the change of pine needle polyprenols’absorbance,the stability is better,therefore,the conservation of pine needle polyprenols should be under 30℃;the illumination make an effect on pine needle polyprenols stability,which should be conserved on darkness;the pine needle polyprenols is sensitivity on different pH : strong acid and strong alkali is notability to pine needle polyrenols,pine needle polyprenols is stability on neutral or weak acid and alkali.The effect of metal ions on pine needle polyprenols:the effect of pine needle polyprenols stability is little by Ca~(2+),Cu~(2+),Al~(3+),Zn~(2+),K~+,Mg~(2+);the effect of pine needle polyprenols stability is much notability by Fe~(3+),Fe~(2+),Ag~+.
The polyprenols is belong to lipoids,whose acid value,iodine value and saponification value of pine needle polyprenols is 3.89 mg KOH/g,2.65 mg KOH/g,2.06 mg KOH/g;The clearance of pine needle polyprenols is up to 23.1% by the method of pyrogallol auto-oxidation.
引文
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