CN115417443B - 一种纳米氧化铈颗粒及其绿色合成工艺和应用 - Google Patents
一种纳米氧化铈颗粒及其绿色合成工艺和应用 Download PDFInfo
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Abstract
本发明公开了一种纳米氧化铈颗粒及其绿色合成工艺和应用,该纳米氧化铈颗粒的制备包括植物提取液制备和纳米氧化铈合成,所述的植物为车前草或白车轴草。该制备方法绿色无污染,设备要求低,便于大规模推广。本发明方法制备得到的纳米氧化铈颗粒可在制备抗PPRSV的兽药中应用,显著拓展了医药新用途。
Description
技术领域
本发明属于新兽药技术领域,具体涉及一种纳米氧化铈颗粒的绿色合成工艺及其应用。
背景技术
稀土元素由于其独特的物理化学特性,具有很好的抗菌、消炎甚至抗病、抗氧化的功效。近些年,一些新的稀土配合物还不断被合成并应用于人体健康、医药领域中。铈是地壳中含量最高的稀土元素,氧化铈纳米粒子是重要的抗菌材料之一,对正常细胞毒性低。
车前草是一种常见中药,具有广泛的药用价值,主要有黄酮类、苯乙酰咖啡酰糖酯类、环烯醚萜类、三萜类等化学成分,并具有抗炎、抗菌、抗溃疡、抗氧化等药理作用,有很好的研发前景。
白车轴草是一种多年生的野生草本植物,产于中国的华北和东北与云南等地,全草可人药,味微甘,性平,具有清热凉血,安神镇痛,祛痰止咳的功效。国外临床试验报道,白车轴草花的酊剂可用于治疗感冒,全草酊剂具收敛止血作用,用作外伤的止血和促进创伤愈合的药物。还发现其所含的异黄酮类物质具有抗癌作用。从白车轴草中提取的大分子物质多糖,具有提高免疫力,抗肿瘤,抗衰老,降血脂等一系列药用和保健功能。
目前大多数制备纳米金属的技术运用的是化学法、物理法,对环境都具有一定的破坏作用。
发明内容
本发明克服上述不足之处,利用绿色植物提取液还原法制备纳米铈颗粒(优选植物为车前草或白车轴草),并对其抗病毒效果进行研究,筛选出畜禽常见兽医病原PRRSV作为测试对象,发现纳米铈对PRRSV有较好的体外抗病毒效果,为新型兽用产品研发提供科学有效的指导。
本发明的目的是通过以下方式实现的:
一种纳米氧化铈颗粒,该氧化铈颗粒是通过以下方法制备得到的:
(1)植物提取液制备:将干燥的植物剪碎,精确称取植物2.5~150g,加入500mL超纯水,歇式加热煮沸60min后得到提取液,冷却至室温,先用快速滤纸初步过滤,再用0.45μm尼龙膜真空抽滤,收集滤液并用超纯水补齐至500mL,4℃冷藏;
(2)纳米氧化铈合成:按体积比1:1~1:10的比例,将三氯化铈溶液与步骤(1)制备得到的植物提取液充分混合,辅助加热,沸腾则暂停加热,待冷却后继续加热,持续60min后,溶液冷却至室温,离心,弃去上清液,收集沉淀,再在280~400℃灼烧2~6h。
所述的植物为车前草或白车轴草,该植物提取液能够有效作为还原剂和封端剂将三氯化铈进行还原,从原子状态合成纳米级颗粒。
优选步骤(1)中称取植物100~150g。
优选按体积比1:1~1:5的比例,将三氯化铈溶液与步骤(1)制备得到的植物提取液充分混合。
步骤(2)所述的三氯化铈溶液浓度为0.001~0.1mol/L。优选为0.1mol/L。
步骤(2)所述的离心是采用8000~10000r/min离心10~30min。
步骤(1)中歇式加热采用电磁炉。本发明采用水作为助溶剂,利用间歇式加热煮沸法,不仅提高了提取效率而且保持了大部分化合物的活性;
步骤(2)中辅助加热采用微波炉。采用加热辅助合成,提高了反应速率,并取得了良好的颗粒分散效果。
步骤(2)中灼烧采用马弗炉。高温灼烧将大部分剩余有机物杂质去除,获得了较为纯净的纳米氧化铈粉末。
上述纳米氧化铈颗粒的制备方法包括以下步骤:
(1)植物提取液制备:将干燥的植物剪碎,精确称取2.5~150g,加入500mL超纯水,歇式加热煮沸60min后得到提取液,冷却至室温,先用快速滤纸初步过滤,然后用0.45μm尼龙膜真空抽滤,收集滤液并用超纯水补齐至500mL,4℃冷藏;
(2)纳米氧化铈合成:按体积比1:1~1:10的比例,将三氯化铈溶液与步骤(1)制备得到的植物提取液充分混合,辅助加热,沸腾则暂停加热,待冷却后继续加热,持续60min后,溶液冷却至室温,离心,弃去上清液,收集沉淀,再在280~400℃灼烧2~6h。
上述纳米氧化铈颗粒可在制备抗PPRSV的兽药中应用。
与现有技术比较本发明的有益效果:
1、绿色无污染,目前合成纳米氧化铈多数采用的水热合成法,往往要添加盐酸或碱液调节反应pH,添加乙醇、聚乙烯吡咯烷酮等有机溶剂作为分散剂,甚至还须添加表面活性剂以获得均一形貌。这些化学试剂均会产生残留,对环境造成不良影响。本发明采用随处可见且价格低廉的药用植物车前草或白车轴草作为原材料,能够有效作为还原剂和封端剂将三氯化铈进行还原,不仅安全无毒,而且还有丰富的药用成分;反应溶剂为纯水,对环境无任何影响。
2、设备要求低,便于大规模推广。现有技术采用高温反应釜容器反应,对设备投入以及操作人员有较高需求,本发明采用普通家用微波炉即可加速反应合成,便于规模化生产。
3、对正常细胞毒性低,拓展了医药新用途。目前主要将纳米氧化铈用于VOCs催化降解、汽车尾气净化、紫外光屏蔽等多方面,但在抗微生物用途方面尚未发现。
附图说明
图1为实施例1车前草提取液合成的纳米氧化铈透射电镜图。
图2为实施例1车前草提取液合成的纳米氧化铈扫描电镜图(选点1)。
图3为实施例1车前草提取液合成的纳米氧化铈点1X射线能谱扫描图。
图4为实施例1车前草提取液合成的纳米氧化铈扫描电镜图(选点2)。
图5为实施例1车前草提取液合成的纳米氧化铈点2X射线能谱扫描图。
图6为实施例1车前草提取液合成的纳米氧化铈X晶体衍射分析图。
其中,X晶体衍射结果表明主要成分为立方体结构的CeO2,平均粒径为5.16±0.94nm。
图7为实施例2白车轴草提取液合成的纳米氧化铈透射电镜图。
图8为实施例2白车轴草提取液合成的纳米氧化铈扫描电镜图(选点1)。
图9为实施例2白车轴草提取液合成的纳米氧化铈点1X射线能谱扫描图。
图10为实施例2白车轴草提取液合成的纳米氧化铈扫描电镜图(选点2)。
图11为实施例2白车轴草提取液合成的纳米氧化铈点2X射线能谱扫描图。
图12为实施例2白车轴草提取液合成的纳米氧化铈X晶体衍射分析图。
其中,X晶体衍射结果表明主要成分为立方体结构的CeO2,平均粒径为18.65±3.53nm。
具体实施方式
以下通过具体实施例对本发明进行进一步的解释说明:
实施例1:
1).植物提取液制备:将干燥的植物剪碎,精确称取150g车前草置于1L洁净烧杯中,然后加入500mL超纯水,倒入烧杯中,用电磁炉(C21-SDHCB9E10,苏泊尔)调p7档间歇式加热煮沸60min;待提取液冷却到室温时,先用18cm快速滤纸(GB/T1914-2007)初步过滤,然后用0.45μm尼龙膜真空抽滤,随后收集滤液并用超纯水补齐至500mL,放入4℃冰箱保存。2).纳米氧化铈合成:按体积比1:1的比例,将预先配好的0.1mol/L三氯化铈溶液100mL与此前制备的车前草提取液100mL充分混合,随后采用微波炉(P70D20TL-D4,格兰仕)辅助加热;观察溶液是否沸腾,如沸腾则暂停加热,待冷却后继续加热,反应持续60min。溶液冷却到室温后,采用10000r/min离心10min,弃去上清液,收集沉淀,转移到马弗炉400℃灼烧2h。
表1 车前草提取液合成的纳米氧化铈点1X射线能谱扫描元素组成分析
表2 车前草提取液合成的纳米氧化铈点2X射线能谱扫描元素组成分析
实施例2:
1)植物提取液制备:
将干燥的植物剪碎,精确称取100g白车轴草置于1L洁净烧杯中,然后加入500mL超纯水,倒入烧杯中,用电磁炉(C21-SDHCB9E10,苏泊尔)调p7档间歇式加热煮沸60min得到提取液;待提取液冷却到室温时,先用18cm快速滤纸(GB/T1914-2007)初步过滤,然后用0.45μm尼龙膜真空抽滤,随后收集滤液并用超纯水补齐至500mL,放入4℃冰箱保存。
2)纳米氧化铈合成:
按体积比1:5的比例,将预先配好的0.1mol/L三氯化铈溶液100mL与此前制备的白车轴草提取液500mL充分混合,随后采用微波炉(P70D20TL-D4,格兰仕)辅助加热;观察溶液是否沸腾,如沸腾则暂停加热,待冷却后继续加热,反应持续60min。溶液冷却到室温后,采用10000r/min离心10min,弃去上清液,收集沉淀,转移到马弗炉400℃灼烧2h。
表3 白车轴草提取液合成的纳米氧化铈点1X射线能谱扫描元素组成分析
表4 白车轴草提取液合成的纳米氧化铈点2X射线能谱扫描元素组成分析
实施例3
体外抗PPRSV效果测定
Marc-145细胞培养、PRRSV SH1705病毒扩增、药物细胞最大安全浓度测定具体参照刘云等[1]的文献报道;不同浓度纳米氧化铈的配制则采用含DMSO的DMEM溶解并结合超声波助溶的方法,具体操作详见Ghaffari等[2]的研究;细胞与药物和病毒的相互作用方式主要有以下3种:(1)直接灭活①将200TCID50病毒稀释液与不同浓度纳米氧化铈溶液(起始浓度为2倍最大安全浓度)按1:1体积比混合;②向铺满底部的单层细胞中按100μL/孔加入药毒混合物(平底96孔细胞培养板,Corning)在37℃共浴4h;③弃上清,PBS清洗细胞两遍,再向每孔细胞中添加100μL含2%FBS的DMEM培养基。(2)阻断作用①向细胞中按每孔100μL加入100TCID50病毒稀释液,在37℃培养2h;②弃上清,PBS清洗细胞两遍,去除未被吸附的病毒;③向每孔细胞中加入对应浓度的100μL纳米氧化铈(起始浓度为最大安全浓度)37℃培养4h;④剩余操作参考直接灭活步骤③。(3)预防作用①向细胞中按每孔100μL加入对应浓度的纳米氧化铈(起始浓度为最大安全浓度),37℃孵育4h;②弃上清,PBS洗细两遍,接着向每孔细胞中加入100μL TCID50病毒稀释液37℃孵育2h;③剩余操作同直接灭活步骤③。共设4个浓度,每浓度8孔重复,每块细胞板上还须要设置正常细胞对照与病毒对照,每组实验重复3次。所有细胞均置于37℃,5%CO2培养箱中培养,每天镜检观察细胞病变情况,待病毒对照组病变率达80~90%时,采用MTT比色法[3]测定细胞的存活率,细胞保护率计算公式[4]如下:
不同剂量处理方式下按照实施例1方法绿色合成纳米氧化铈颗粒对PRRSV的抑制率(%)
剂量(mg/mL) | 抑制 | 阻断作用 | 灭活 |
5 | 19.19078947 | 43.80680221 | 42.09098497 |
2.5 | 7.736842105 | 37.65108217 | 59.52003339 |
1.25 | 10.90460526 | 36.42368594 | 62.99248748 |
0.625 | -0.753289474 | 33.24276211 | 61.88230384 |
纳米氧化铈细胞最大安全浓度为5mg/mL,表明安全性较好,此外灭活等体外抗病毒效果要优于利巴韦林。
参考文献
[1]秦枫,刘云,夏文龙,等.3种半边莲提取物体外抗猪繁殖与呼吸综合征病毒的作用研究[J].河南农业大学学报,2020,54(3):462-470.
[2]Ghaffari H,Tavakoli A,Moradi A,et al.Inhibition of H1n1 InfluenzaVirus Infection By Zinc Oxide Nanoparticles:Another Emerging Application ofNanomedicine[J].Journal of Biomedical Science,2019,26(1):1-10.
[3]Levi R,Beeor-tzahar T,Arnon R.Microculture Virus Titration--aSimple Colourimetric Assay for Influenza Virus Titration.[J].Journal ofVirological Methods,1995,52(1):55-64.
[4]R soleimani E,Mt K.In Vitro Antiviral Effect Of"Nanosilver"onInfluenza Virus[J].Daru-journal of Faculty of Pharmacy,2009,17(2):88-93.
Claims (5)
1.一种纳米氧化铈颗粒在制备抗PPRSV的兽药中的应用;所述的氧化铈颗粒是通过以下方法制备得到的:
(1)植物提取液制备:将干燥的植物剪碎,每2.5~150g植物加入500mL超纯水,歇式加热煮沸60min后得到提取液,冷却至室温,先用快速滤纸初步过滤,再用0.45μm尼龙膜真空抽滤,收集滤液并用超纯水补齐至500mL, 4℃冷藏;所述的植物为车前草或白车轴草;
(2)纳米氧化铈合成:按体积比1:1~1:10的比例,将三氯化铈溶液与步骤(1)制备得到的植物提取液充分混合,辅助加热,沸腾则暂停加热,待冷却后继续加热,持续60min后,溶液冷却至室温,离心,弃去上清液,收集沉淀, 再在280~400℃灼烧2~6h;所述的三氯化铈溶液浓度为0.001~0.1mol/L。
2.根据权利要求1所述的应用,其特征在于步骤(2)所述的离心是采用8000~10000r/min离心10~30min。
3.根据权利要求1所述的应用,其特征在于步骤(1)中歇式加热采用电磁炉。
4.根据权利要求1所述的应用,其特征在于步骤(2)中辅助加热采用微波炉。
5.根据权利要求1所述的应用,其特征在于步骤(2)中灼烧采用马弗炉。
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