CN110314178B - 具有广谱杀菌活性的纯天然复方精油及其制备和用途 - Google Patents
具有广谱杀菌活性的纯天然复方精油及其制备和用途 Download PDFInfo
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- CN110314178B CN110314178B CN201810585521.6A CN201810585521A CN110314178B CN 110314178 B CN110314178 B CN 110314178B CN 201810585521 A CN201810585521 A CN 201810585521A CN 110314178 B CN110314178 B CN 110314178B
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- volatile oil
- oil
- rhizoma atractylodis
- compound essential
- essential oil
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Abstract
本发明公开了一种具有广谱杀菌活性的纯天然复方精油的制备和用途,该复方精油由从菊科苍术属植物茅苍术或北苍术的干燥根、茎以及樟科植物肉桂的干燥嫩枝或树皮中提取挥发油后进行混合复配获得,其中,两种挥发油的体积含量为:苍术挥发油:40‑70份,桂枝挥发油:30‑60份。该复方精油能对金黄色葡萄球菌、大肠杆菌及白色念珠菌具有很强的杀灭作用。
Description
技术领域
本发明属于杀菌、消毒、防腐技术领域,具体涉及纯天然复方精油及其制备方法和在医疗药品、卫生消毒产品、食品防腐和日用品方面的用途。
背景技术
苍术(Rhizoma Atractylodis)又名赤术,为菊科苍术属植物茅苍术Atractylodeslancea(Thunb.)DC.或北苍术Atractylodeschinensis(DC.)Koidz.的干燥根茎,南苍术又称茅苍术。味辛性温、专入脾胃、以燥湿健脾、祛风除湿为主要功能。用苍术熏蒸空气,具有解郁避秽的作用,其主要杀菌活性成分为挥发油。苍术烟熏消毒应用于病房、产房、手术室等取得满意效果。桂枝为樟科植物肉桂(Cinnamonum cassia Presl.)的干燥嫩枝,具有发汗解肌,温通经脉,助阳化气,平冲降气的功效。桂枝挥发油为桂枝的挥发性成分,是桂枝的主要活性物质,现代研究发现桂枝挥发油是桂枝的主要有效部位,具有良好的抗炎、抗菌、抗病毒和抗肿瘤等作用。苍术挥发油和桂枝挥发油单独的杀菌活性均有文献报道,而由苍术和桂枝挥发油制备的复方精油的杀菌活性、提取制备方法及用途未见相关文献及专利。单一的苍术挥发油或桂枝挥发油不能同时杀灭金黄色葡萄球菌、大肠杆菌及白色念珠菌并使最终杀菌效果达到5个对数值的国家卫生消毒标准,而本发明的纯天然复方精油可以发挥两种精油的协同增效作用,同时杀灭金黄色葡萄球菌、大肠杆菌及白色念珠菌并使最终杀菌效果达到且高于5个对数值的国家卫生消毒标准。
发明内容
本发明的目的是提供一种具有广谱抗菌活性的纯天然复方精油的制备和用途,该复方精油从菊科苍术属植物茅苍术或北苍术的干燥根、茎以及樟科植物肉桂的干燥嫩枝或树皮中提取挥发油后进行混合复配获得。
具体情况下,复方精油中两种挥发油的体积含量为:苍术挥发油:40-70份,桂枝挥发油:30-60份。
进一步优选情况下,两种挥发油的体积含量为:苍术挥发油:50-60份,桂枝挥发油:40-50份。
苍术挥发油主要含有β-桉油醇、苍术素、苍术酮、苍术醇、榄香油醇等挥发性物质。不仅能够对空气中的结核分枝杆菌、铜绿假单胞菌等有一定的杀灭作用,还对大肠杆菌和金黄色葡萄球菌有很强的杀灭作用。桂枝油主要含有苯甲醛、苯丙醛、反式桂皮醛、桂皮醛等挥发性物质,具有显著的抗菌、镇静、镇痛等效果。苍术和桂枝作为常用中药,其作用效果在古代早有记载。然而发明人在大量实验中首次发现,有着相同特质的精油当被以合适的比例配比时,会产生协同增效作用,使杀菌效力倍增,即1+1大于2的效果,因此,发明人在充分挖掘药用植物的各种特性和功效的基础上,经过主辅搭配、设计了苍术与桂枝挥发油的纯天然杀菌复方精油。
该复方精油杀菌在于苍术挥发油中的主要活性成分苍术醇等和桂枝挥发油中的主要活性成分桂皮醛等具有协同作用,二者合用降低用量的同时能对金黄色葡萄球菌、大肠杆菌及白色念珠菌具有很强的杀灭作用,其机理在于苍术醇和桂皮醛协同抑制细菌细胞壁合成,胞壁粘肽合成酶(包括转肽酶、羧胎酶、内肽酶),从而阻碍细胞壁肽聚糖的合成,使细胞壁缺损,菌体破裂死亡。
本发明的复方精油,可以通过水蒸气蒸馏法制得,具体包括以下步骤:
(1)苍术油提取:将苍术根茎粉碎成干粉,装入盛有10倍量水的水蒸气蒸馏提取器中,温度控制在100℃附近(±5℃),待提取器支管中流下的液体为无色时,即停止提取,用分液漏斗去除下部蒸馏水即得油状粗提物,密封后置于4℃冰箱保存备用;
(2)桂枝油提取:将桂枝粉碎成干粉,装入盛有12倍量水的水蒸气蒸馏提取器中,温度控制在100℃附近(±5℃),待提取器支管中流下的液体为无色时,即停止提取用分液漏斗去除下部蒸馏水即得油状粗提物,密封后置于4℃冰箱保存备用;
(3)将苍术油和桂枝油按一定比例进行混合,即得具有广谱抗菌活性的纯天然复方精油。
另外,本发明中的苍术合桂枝挥发油,也可通过CO2超临界(或亚临界)流体提取法制得,具体包括以下步骤:
(1)苍术油提取:将苍术根茎粉碎成干粉,置入适当大小的CO2超临界流体提取罐中,直接用超临界CO2进行提取,即得;
(2)桂枝油提取:将桂枝粉碎成干粉,置入适当大小的CO2超临界流体提取罐中,直接用超临界CO2进行提取,即得;
(3)将苍术油和桂枝油按一定比例进行混合,即得具有广谱抗菌活性的纯天然复方精油。
根据本发明的优选方面,还提供了一种三组分复方精油及其制备方法,该方法包括:
(1)苍术油提取:将苍术根茎粉碎成干粉,装入盛有10倍量水的水蒸气蒸馏提取器中,温度控制在100℃附近(±5℃),待提取器支管中流下的液体为无色时,即停止提取,用分液漏斗去除下部蒸馏水即得油状粗提物,密封后置于4℃冰箱保存备用;
(2)桂枝油提取:将桂枝粉碎成干粉,装入盛有12倍量水的水蒸气蒸馏提取器中,温度控制在100℃附近(±5℃),待提取器支管中流下的液体为无色时,即停止提取,用分液漏斗去除下部蒸馏水即得油状粗提物,密封后置于4℃冰箱保存备用;
(3)药曲草油提取工艺:将药曲草粉碎成干粉,装入盛有15倍量水的水蒸气蒸馏提取器中,温度控制在100℃附近(±5℃),待提取器支管中流下的液体为无色时,即停止提取,用分液漏斗去除下部蒸馏水即得油状粗提物,密封后置于4℃冰箱保存备用。
将上述制备的苍术油和药曲草油按照10:1至10:3体积比进行混合,优选10:2体积比进行混合,形成第一混合油。
将第一混合油60‐80℃、优选70℃水浴加热10至30分钟后加入桂枝油形成第二混合油,其中所加入的桂枝油与第一混合液的体积比为1:3至3:1之间,优选为1:2。
再将第二混合油在50‐60℃,优选55℃水浴加热5至10分钟,从而制得改良三组分复方精油。
发明人在配伍试验时首次发现,以上述工艺步骤加入的药曲草油可以对苍术合桂枝挥发油的杀菌效果进行显著改良,这可能与其渗透性能所带来的协同效应有关,还可能与其辅助杀菌性能也有关。
本发明对上述复方精油(包括两组分和三组分复方精油,下同)进行杀菌实验,表明对金黄色葡萄球菌、大肠杆菌及白色念珠菌等均有很强的杀菌活性。
本发明中的复方精油可单独使用,可用于制备治疗或缓解细菌性或不明原因之发炎、发热、疼痛等症状的药物(包括人用和动物用药品)。
本发明中的复方精油也可以配伍其它具抗菌消炎、解热镇痛作用的中药,如金银花、黄芩、连翘、蒲公英等,或西药青霉素、罗红霉素、头孢霉素等,制成具有抗菌消炎、解热镇痛作用的口服、注射等内用制剂,或栓剂、软膏、喷雾剂、滴剂等外用制剂,用于治疗和缓解各种感染性疾病或无名肿毒所致的发炎、发热、疼痛等症状。
本发明中的复方精油还可用于杀菌日用品的开发。
本发明中的复方精油也可以添加一些表面活性剂和辅料,如TEA十二烷基硫酸钠、椰油酰胺DEA、椰油酰胺MEA、月桂基醚硫酸钠等,开发包括消杀剂、消毒湿巾、口腔抑菌喷雾剂、衣物消毒液、杀菌牙膏、抑菌沐浴液等日用产品。
本发明中的复方精油还可用于食品和保健食品中的纯天然杀菌防腐剂。
本发明中的复方精油还可用于家禽、畜牧、水产养殖等的纯天然杀菌消毒产品的开发。
本发明原料来源广、成本低、毒性小,制备方法简单、通用,产品具有广谱抗菌消炎、解热镇痛效果。
具体实施方式
一、复方精油的制备
制备工艺(1)
苍术油提取工艺:将苍术根茎粉碎成干粉,装入盛有10倍量水的水蒸气蒸馏提取器中,温度控制在100℃附近,待提取器支管中流下的液体为无色时,约6h,即停止提取,用分液漏斗去除下部蒸馏水即得油状粗提物,密封后置于4℃冰箱保存备用。
桂枝油提取工艺:将桂枝粉碎成干粉,装入盛有12倍量水的水蒸气蒸馏提取器中,温度控制在100℃附近,待提取器支管中流下的液体为无色时,约6h,即停止提取,用分液漏斗去除下部蒸馏水即得油状粗提物,密封后置于4℃冰箱保存备用。
将苍术油和桂枝油按一定比例进行混合,即得具有广谱抗菌活性的两组分纯天然复方精油。
制备工艺(2)
药曲草油提取工艺:将药曲草(透骨草)粉碎成干粉,装入盛有15倍量水的水蒸气蒸馏提取器中,温度控制在100℃附近,待提取器支管中流下的液体为无色时,约6h,即停止提取,用分液漏斗去除下部蒸馏水即得油状粗提物,密封后置于4℃冰箱保存备用。
将上述制备的苍术油和药曲草油按照10:1至10:3体积比进行混合,优选10:2体积比进行混合,形成第一混合油。
将第一混合油60‐80℃、优选70℃水浴加热10至30分钟后加入桂枝油形成第二混合油,其中所加入的桂枝油与第一混合液的体积比为1:3至3:1之间,优选为1:2。
再将第二混合油在50‐60℃,优选55℃水浴加热5至10分钟,从而制得改良的具有广谱抗菌活性的三组分纯天然复方精油。
二、杀菌试验
试验1
(1)选择金黄色葡萄球菌、大肠杆菌、白色念株菌三种菌株分别按消毒技术规范配制实验用菌悬液,浓度为1×108cfu/ml~5×108cfu/ml。
(2)取0.2589g不同混合比的复方精油溶于5mL乙醇中,用蒸馏水定容至25mL,制成消毒液,浓度为1.0%。
(3)取消毒试验用无菌大试管,先加入0.5ml试验用菌悬液,再加入0.5ml有机干扰物质,混匀,置20℃±1℃水浴中5min后,用无菌吸管吸取消毒液4.0ml注入其中,迅速混匀并立即记时。
(4)待试验菌与消毒液相互作用至各预定时间,分别吸取0.5ml试验菌与消毒液混合液加于4.5ml经灭菌的中和剂中,混匀。
(5)各管试验菌与消毒液混合液经加中和剂作用10min后,分别吸取1.0ml样液,按活菌培养计数方法测定存活菌数,每管样液接种2个平皿即可。如平板上生长的菌落数较多时,可进行系列10倍稀释后,再进行活菌培养计数。
(6)同时用稀释液代替消毒液,进行平行试验,作为阳性对照。
(7)所有试验样本均在37℃温箱中培养,对细菌繁殖体培养48h观察最终结果;对细菌芽孢需培养72h观察最终结果。
(8)试验重复3次,计算各组的活菌浓度(cfu/ml),并换算为对数值(N),然后按下式计算杀灭对数值:
杀灭对数值(KL)=对照组平均活菌浓度的对数值(No)-试验组活菌浓度对数值(Nx)
试验结果如表1所示。
表1:悬液定量杀菌试验结果
从以上杀菌试验结果表明:
苍术油和桂枝油单独使用对金黄色葡萄球菌具有较强的杀灭作用,杀灭对数值(KL)>5.0,但对大肠杆菌和白色念珠菌的杀灭对数值达不到使用效果。两者合用后从实例3-6的筛选结果来看,苍术挥发油和桂枝挥发油中的主要活性成分产生了协同作用,降低用量的同时能对金黄色葡萄球菌、大肠杆菌及白色念珠菌具有明显的抑制作用,综合平均杀灭对数值分别为5.91、5.75、5.76和5.85。
试验2
将上述制备工艺(1)制备的两组分复方精油与制备工艺(2)制备的三组分复方精油按照上述试验1的标准进行杀菌试验,其中药曲草油按照表2所列体积份额外加入,试验结果如下表2所示。
表2:悬液定量杀菌试验结果
表2杀菌试验结果表明:
制备工艺(2)制备的改良的三组分复方精油的杀菌效果得到显著加强,这与以上述特定工艺步骤加入的药曲草油将二者的杀菌作用进一步促进整合有关。
三、具体应用示例
实施例1两组分复方精油软胶囊的制备
配方(重量比):两组分复方精油5.8%,软胶囊基质:明胶17.7%、琼脂17.7%、去离子水58.8%。
制法:将上述软胶囊基质置于化胶罐中配成胶液后,用软胶囊机压制成软胶囊,控制每粒丸重0.5g,即得两组分复方精油胶囊1000粒。
实施例2两组分复方精油栓剂的制备
配方(重量比):两组分复方精油5.9%,冰片1.2%,栓剂基质:聚氧乙烯硬脂酸脂88.5%、聚山梨酯80 4.4%。
制法:先将冰片以适量乙醇溶解,然后与两组分复方精油、聚山梨酯80充分混匀。另将聚氧乙烯硬脂酸脂置水浴上熔化,加入上述药液,充分搅匀,灌入栓剂模中,冷却后取出,制成1000粒,即得。
实施例3改良三组分复方精油软胶囊的制备
配方(重量比):三组分复方精油5.8%,软胶囊基质:明胶17.7%、琼脂17.7%、去离子水58.8%。
制法:将上述软胶囊基质置于化胶罐中配成胶液后,用软胶囊机压制成软胶囊,控制每粒丸重0.5g,即得三组分复方精油胶囊1000粒。
上述软胶囊和栓剂可用于治疗和缓解细菌性或不明原因所致***、肾炎、膀胱炎、***炎、乳腺炎、扁桃体炎、肺炎、脑炎、腮腺炎、上呼吸道感染等疾病之发炎、发热、疼痛等症状,有良好的应用前景。
Claims (3)
1.一种具有广谱杀菌活性的纯天然复方精油,该复方精油由通过水蒸气蒸馏法或通过CO2超临界流体提取法从菊科苍术属植物茅苍术或北苍术的干燥根、茎中提取的挥发油与樟科植物肉桂的干燥嫩枝或树皮中提取的挥发油进行混合复配后获得,其中,两种挥发油的体积含量为:苍术挥发油:40-70份,桂枝挥发油:30-60份,
其中通过水蒸气蒸馏法制备苍术挥发油和桂枝挥发油如下:
将苍术根茎粉碎成干粉,装入盛有10倍量水的水蒸气蒸馏提取器中,温度控制在100℃附近,待提取器支管中流下的液体为无色时,即停止提取,用分液漏斗去除下部蒸馏水即得油状粗提物——苍术挥发油,密封后置于4℃冰箱保存备用;
将桂枝粉碎成干粉,装入盛有12倍量水的水蒸气蒸馏提取器中,温度控制在100℃附近,待提取器支管中流下的液体为无色时,即停止提取用分液漏斗去除下部蒸馏水即得油状粗提物——桂枝挥发油,密封后置于4℃冰箱保存备用,
其中通过CO2超临界流体提取法制备苍术挥发油和桂枝挥发油如下:
将苍术根茎粉碎成干粉,置入适当大小的CO2超临界流体提取罐中,直接用超临界CO2进行提取,即得苍术挥发油;
将桂枝粉碎成干粉,置入适当大小的CO2超临界流体提取罐中,直接用超临界CO2进行提取,即得桂枝挥发油。
2.根据权利要求1所述的复方精油在制备消杀剂或杀菌日用产品中的应用。
3.根据权利要求1所述的复方精油在制备人用或兽用消毒产品中的应用。
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