CN116750726B - 一种PtCuTe纳米材料及其制备方法和修复凝胶 - Google Patents
一种PtCuTe纳米材料及其制备方法和修复凝胶 Download PDFInfo
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- CN116750726B CN116750726B CN202311024863.8A CN202311024863A CN116750726B CN 116750726 B CN116750726 B CN 116750726B CN 202311024863 A CN202311024863 A CN 202311024863A CN 116750726 B CN116750726 B CN 116750726B
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- tellurite
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- platinum
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- 238000002360 preparation method Methods 0.000 title abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 7
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 6
- SITVSCPRJNYAGV-UHFFFAOYSA-L tellurite Chemical compound [O-][Te]([O-])=O SITVSCPRJNYAGV-UHFFFAOYSA-L 0.000 claims description 42
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 22
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 12
- 239000010949 copper Substances 0.000 claims description 12
- 229910052700 potassium Inorganic materials 0.000 claims description 12
- 239000011591 potassium Substances 0.000 claims description 12
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- -1 copper tetrafluoroborate Chemical compound 0.000 claims description 11
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 9
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 8
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 8
- 239000003223 protective agent Substances 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- 229910052788 barium Inorganic materials 0.000 claims description 6
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 6
- ODWXUNBKCRECNW-UHFFFAOYSA-M bromocopper(1+) Chemical compound Br[Cu+] ODWXUNBKCRECNW-UHFFFAOYSA-M 0.000 claims description 6
- BFPJYWDBBLZXOM-UHFFFAOYSA-L potassium tellurite Chemical compound [K+].[K+].[O-][Te]([O-])=O BFPJYWDBBLZXOM-UHFFFAOYSA-L 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 6
- 239000004332 silver Substances 0.000 claims description 6
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- 239000011734 sodium Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- KLFRPGNCEJNEKU-FDGPNNRMSA-L (z)-4-oxopent-2-en-2-olate;platinum(2+) Chemical compound [Pt+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O KLFRPGNCEJNEKU-FDGPNNRMSA-L 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 4
- ZKXWKVVCCTZOLD-UHFFFAOYSA-N copper;4-hydroxypent-3-en-2-one Chemical compound [Cu].CC(O)=CC(C)=O.CC(O)=CC(C)=O ZKXWKVVCCTZOLD-UHFFFAOYSA-N 0.000 claims description 4
- QYCVHILLJSYYBD-UHFFFAOYSA-L copper;oxalate Chemical compound [Cu+2].[O-]C(=O)C([O-])=O QYCVHILLJSYYBD-UHFFFAOYSA-L 0.000 claims description 4
- NQNFKQOIDNMNBB-UHFFFAOYSA-L dichloroplatinum;triphenylphosphane Chemical compound Cl[Pt]Cl.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NQNFKQOIDNMNBB-UHFFFAOYSA-L 0.000 claims description 4
- FWBOFUGDKHMVPI-UHFFFAOYSA-K dicopper;2-oxidopropane-1,2,3-tricarboxylate Chemical compound [Cu+2].[Cu+2].[O-]C(=O)CC([O-])(C([O-])=O)CC([O-])=O FWBOFUGDKHMVPI-UHFFFAOYSA-K 0.000 claims description 4
- LMABILRJNNFCPG-UHFFFAOYSA-L ethane-1,2-diamine;platinum(2+);dichloride Chemical compound [Cl-].[Cl-].[Pt+2].NCCN LMABILRJNNFCPG-UHFFFAOYSA-L 0.000 claims description 4
- FXADMRZICBQPQY-UHFFFAOYSA-N orthotelluric acid Chemical compound O[Te](O)(O)(O)(O)O FXADMRZICBQPQY-UHFFFAOYSA-N 0.000 claims description 4
- VBWYZPGRKYRKNV-UHFFFAOYSA-N 3-propanoyl-1,3-benzoxazol-2-one Chemical compound C1=CC=C2OC(=O)N(C(=O)CC)C2=C1 VBWYZPGRKYRKNV-UHFFFAOYSA-N 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- AOFZMTDNRXMXOR-UHFFFAOYSA-L Cl[Pt](Cl)C1=CC=CC=C1 Chemical compound Cl[Pt](Cl)C1=CC=CC=C1 AOFZMTDNRXMXOR-UHFFFAOYSA-L 0.000 claims description 3
- OCUCCJIRFHNWBP-IYEMJOQQSA-L Copper gluconate Chemical compound [Cu+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O OCUCCJIRFHNWBP-IYEMJOQQSA-L 0.000 claims description 3
- 229910021594 Copper(II) fluoride Inorganic materials 0.000 claims description 3
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- NOWPEMKUZKNSGG-UHFFFAOYSA-N azane;platinum(2+) Chemical compound N.N.N.N.[Pt+2] NOWPEMKUZKNSGG-UHFFFAOYSA-N 0.000 claims description 3
- GAGXPIXDGRGRSX-UHFFFAOYSA-N azane;tellurous acid Chemical compound [NH4+].[NH4+].[O-][Te]([O-])=O GAGXPIXDGRGRSX-UHFFFAOYSA-N 0.000 claims description 3
- KLNFSAOEKUDMFA-UHFFFAOYSA-N azanide;2-hydroxyacetic acid;platinum(2+) Chemical compound [NH2-].[NH2-].[Pt+2].OCC(O)=O KLNFSAOEKUDMFA-UHFFFAOYSA-N 0.000 claims description 3
- VSRXQHXAPYXROS-UHFFFAOYSA-N azanide;cyclobutane-1,1-dicarboxylic acid;platinum(2+) Chemical compound [NH2-].[NH2-].[Pt+2].OC(=O)C1(C(O)=O)CCC1 VSRXQHXAPYXROS-UHFFFAOYSA-N 0.000 claims description 3
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- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 3
- GKMPTXZNGKKTDU-UHFFFAOYSA-L cadmium(2+);tellurite Chemical compound [Cd+2].[O-][Te]([O-])=O GKMPTXZNGKKTDU-UHFFFAOYSA-L 0.000 claims description 3
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- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 3
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- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
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- 229920002518 Polyallylamine hydrochloride Polymers 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 102000019197 Superoxide Dismutase Human genes 0.000 description 1
- 108010012715 Superoxide dismutase Proteins 0.000 description 1
- 229920004890 Triton X-100 Polymers 0.000 description 1
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- 238000002835 absorbance Methods 0.000 description 1
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- 239000007864 aqueous solution Substances 0.000 description 1
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- 239000012620 biological material Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
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- VUBLMKVEIPBYME-UHFFFAOYSA-N carbon monoxide;osmium Chemical group [Os].[Os].[Os].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-] VUBLMKVEIPBYME-UHFFFAOYSA-N 0.000 description 1
- NQZFAUXPNWSLBI-UHFFFAOYSA-N carbon monoxide;ruthenium Chemical group [Ru].[Ru].[Ru].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-] NQZFAUXPNWSLBI-UHFFFAOYSA-N 0.000 description 1
- FQNHWXHRAUXLFU-UHFFFAOYSA-N carbon monoxide;tungsten Chemical group [W].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-] FQNHWXHRAUXLFU-UHFFFAOYSA-N 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
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- XRWMGCFJVKDVMD-UHFFFAOYSA-M didodecyl(dimethyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCC XRWMGCFJVKDVMD-UHFFFAOYSA-M 0.000 description 1
- QFEOTYVTTQCYAZ-UHFFFAOYSA-N dimanganese decacarbonyl Chemical group [Mn].[Mn].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-] QFEOTYVTTQCYAZ-UHFFFAOYSA-N 0.000 description 1
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- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 description 1
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- 229910021645 metal ion Inorganic materials 0.000 description 1
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- 229910052759 nickel Inorganic materials 0.000 description 1
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- LDVMBMMEPJDZLP-UHFFFAOYSA-N oxirane;styrene Chemical compound C1CO1.C=CC1=CC=CC=C1 LDVMBMMEPJDZLP-UHFFFAOYSA-N 0.000 description 1
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- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 description 1
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- 231100000397 ulcer Toxicity 0.000 description 1
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Abstract
本公开提供了一种PtCuTe纳米材料及其制备方法和修复凝胶,涉及医用配置品技术领域,所述制备方法包括:将Pt的金属前体、Cu的金属前体、Te的金属前体及还原剂均匀分散在溶剂中,得到反应液;将所述反应液转移至反应釜中进行水热反应,反应结束后得到PtCuTe纳米材料。本公开将Pt、Cu、Te有机结合成新型纳米材料,PtCuTe纳米材料不仅对ROS有高效的清除能力,而且还具有良好的ROS非依赖性抗菌性能,可高效促进糖尿病伤口愈合。
Description
技术领域
本公开涉及医用配置品技术领域,尤其涉及一种PtCuTe纳米材料及其制备方法和修复凝胶。
背景技术
糖尿病危害着全球数亿人的健康,慢性不愈合的皮肤溃疡是其严重并发症。溃疡皮肤局部活性氧(Reactive oxygen species, ROS)大量积累、细菌感染、微循环紊乱、长期慢性炎症等导致溃疡迁延不愈。另外,高ROS水平通常会导致局部不可逆的氧化损伤、炎症升高、细菌感染的风险增加。因此高效清除糖尿病伤口中过量ROS是促进伤口愈合的关键。
目前用于清除ROS的材料大多是纳米酶或抗氧化生物材料,这些材料仍然存在ROS清除能力不足或生物安全性低的缺陷。
发明内容
本公开提供了一种PtCuTe纳米材料及其制备方法和修复凝胶,以至少解决现有技术中存在的以上技术问题。
根据本公开的第一方面,提供了一种PtCuTe纳米材料的制备方法,所述方法包括:
将Pt的金属前体、Cu的金属前体、Te的金属前体及还原剂均匀分散在溶剂中,得到反应液;
将所述反应液转移至反应釜中进行水热反应,反应结束后得到PtCuTe纳米材料。
在一可实施方式中,所述反应液中还包括助剂和保护剂,所述主机用于调节还原速度,所述保护剂用于用于防止水热反应过程生成的纳米颗粒体团聚。
在一可实施方式中,所述Pt的金属前体为可溶性Pt盐;所述Cu的金属前体为可溶性Cu盐;所述Te的金属前体为含Te的可溶性化合物。
在一可实施方式中,所述Pt的金属前体包括:乙酰丙酮铂、氯铂酸、氯铂酸钾、氯铂酸铵、四氯合铂四氨合铂酸盐、氯铂酸钠、氯化铂、乙二胺氯化铂、氯亚铂酸、氯亚铂酸钾、氯亚铂酸铵、溴化铂、溴铂酸、碘铂、二亚硝基二氨铂、硝酸铂、四氨合硝酸铂、亚硫酸铂、甲啶铂吡铂、奈达铂、顺铂、卡铂、米铂、依铂、奥沙利铂、二腈苯基二氯化铂、三苯基膦氯化铂中的一种或多种。
在一可实施方式中,所述Cu的金属前体包括:乙酸铜、氯化亚铜、溴化亚铜、碘化亚铜、氟化铜、氯化铜、溴化铜、硫酸铜、硝酸铜、甲酸铜、乙酰丙酮铜、柠檬酸铜、葡萄糖酸铜、甘氨酸铜、环烷酸铜、草酸铜、酞菁铜、四氟硼酸铜中的一种或多种。
在一可实施方式中,所述Te的金属前体包括:碲酸、亚碲酸、亚碲酸锂、亚碲酸钠、亚碲酸钾、亚碲酸钙、亚碲酸锶、亚碲酸钡、亚碲酸镉、亚碲酸铜、亚碲酸银、碲酸钠、原碲酸钠、原碲酸氢钠、碲酸钾、原碲酸氢钾、碲酸铵、碲酸钡、原碲酸铋、碲酸银、原碲酸汞、甲碲醇、乙碲醇、苯碲酚、2,4,6-三甲基苯碲酚、二甲基碲、二(三氟甲基)碲、二苯基二碲、碲半胱氨酸、羰基碲、四碲代硅酸铯、四碲代钒酸亚铜、五氟碲酸、六氯合碲酸钾、三苯基碲化膦、四甲醇碲、四乙醇碲中的一种或多种。
在一可实施方式中,所述助剂为羰基化合物。
在一可实施方式中,所述水热反应的条件为:水热温度140-300℃,水热时间1-24h。
根据本公开的第二方面,提供了一种PtCuTe纳米材料,根据上述所述方法制备得到。
根据本公开的第三方面,提供了一种修复凝胶,包括PtCuTe纳米材料、聚乙烯醇凝胶和水,所述PtCuTe纳米材料的浓度为1-10μg/mL,所述聚乙烯醇凝胶浓度为300-500 mg/mL。
本公开提供的PtCuTe纳米材料,通过将Pt的金属前体、Cu的金属前体、Te的金属前体、还原剂及催化剂均匀分散在溶剂中,得到反应液;再将反应液转移至反应釜中进行水热反应,反应结束后得到PtCuTe纳米材料。将Pt、Cu、Te有机结合成新型纳米材料,PtCuTe纳米材料不仅对ROS有高效的清除能力,而且还具有良好的ROS非依赖性抗菌性能。
应当理解,本部分所描述的内容并非旨在标识本公开的实施例的关键或重要特征,也不用于限制本公开的范围。本公开的其它特征将通过以下的说明书而变得容易理解。
附图说明
通过参考附图阅读下文的详细描述,本公开示例性实施方式的上述以及其他目的、特征和优点将变得易于理解。在附图中,以示例性而非限制性的方式示出了本公开的若干实施方式,其中:
在附图中,相同或对应的标号表示相同或对应的部分。
图1示出了本公开实施例一种PtCuTe纳米材料的制备方法的流程示意图;
图2a示出了本公开实施例1制备的PtCuTe纳米材料的TEM图像(标尺200nm);
图2b示出了本公开实施例1制备的PtCuTe纳米材料的TEM图像(标尺2nm);
图2c示出了本公开实施例1制备的PtCuTe纳米材料的TEM图像(标尺2nm);
图2d为图2c中e处的放大图;
图2e示出了本公开实施例1制备的PtCuTe纳米材料的XRD图谱;
图2f示出了本公开实施例1制备的PtCuTe纳米材料的高角度环形暗场射扫描投射电子显微镜图及元素分布图;
图2g示出了本公开实施例1制备的PtCuTe纳米材料的ICP-AES元素定量分析;
图2h示出了本公开实施例1制备的PtCuTe纳米材料的Pt 4f XPS图谱;
图3示出了本公开实施例1制备的PtCuTe纳米材料催化H2O2氧化TMB的结果示意图;
图4示出了本公开实施例1制备的PtCuTe 纳米材料清除.OH的电子顺磁共振波示意图;
图5示出了本公开实施例1制备的不同浓度PtCuTe 纳米材料清除.OH的效果示意图;
图6a为空白对照组(control)、0.25 μg/mL PtCuTe组、0.50 μg/mL PtCuTe组、1.00 μg/mL PtCuTe组、2.00 μg/mL PtCuTe组金黄色葡萄球菌稀释涂布后的菌落形态图;
图6b为图6a的菌落形成单位定量分析;
图6c为各组金黄色葡萄球菌活体染色;
图6d为各组金黄色葡萄球菌扫描电镜图;
图7a为正常组(NG)、高糖组(HG)、高糖+0.25 μg/mL PtCuTe组 (HG+0.25)、高糖+0.50 μg/mL PtCuTe 组(HG+0.50) 内皮细胞管腔形成实验图;
图7b为各组内皮细胞管腔形成实验图;
图8a为正常组(NG)、高糖组(HG)、高糖+0.25 μg/mL PtCuTe组 (HG+0.25)、高糖+0.50 μg/mL PtCuTe 组(HG+0.50) 成纤维细胞运动轨迹图;
图8b为各组真皮成纤维细胞运动速度;
图8c为运动轨迹长度;
图9a为正常组(NG)、高糖组(HG)、高糖+0.25 μg/mL PtCuTe组 (HG+0.25)、高糖+0.50 μg/mL PtCuTe 组(HG+0.50) 巨噬细胞极化分型流式细胞结果图;
图9b为流式细胞结果;
图9c为流式细胞结果;
图10a为NG组、HG组、HG+ 5.0 μg/mL PtCuTe组小鼠皮肤缺损局部第0、8天形态图及愈合比例模式图;
图10b为各组皮肤愈合百分率折线图。
具体实施方式
为使本公开的目的、特征、优点能够更加的明显和易懂,下面将结合本公开实施例中的附图,对本公开实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本公开一部分实施例,而非全部实施例。基于本公开中的实施例,本领域技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本公开保护的范围。
由于高ROS水平通常会导致伤口局部不可逆的氧化损伤、炎症升高、细菌感染的风险增加,因此高效清除糖尿病伤口中过量ROS是促进伤口愈合的关键。另外由于不同种类细胞,其ROS浓度水平存在异质性,较低的生理水平ROS对维持内皮细胞、成纤维细胞正常生理功能至关重要,而吞噬细胞(巨噬细胞、中性粒细胞)则通过较高水平ROS杀死入侵的病原微生物。因此,在针对糖尿病皮肤溃疡治疗中,若单方面强调高效的ROS清除,则会损害吞噬细胞ROS依赖性的抗菌功能,从而带来不可控制的继发感染。
为了解决该问题,本公开提出具有强ROS清除能力、且具有ROS非依赖性抗菌能力的PtCuTe纳米材料。
如图1所示,一种PtCuTe纳米材料的制备方法,包括如下步骤:
步骤101、将Pt的金属前体、Cu的金属前体、Te的金属前体及还原剂均匀分散在溶剂中,得到反应液。
其中,Pt的金属前体为可溶性铂盐,包括:乙酰丙酮铂、氯铂酸、氯铂酸钾、氯铂酸铵、四氯合铂四氨合铂酸盐、氯铂酸钠、氯化铂、乙二胺氯化铂、氯亚铂酸、氯亚铂酸钾、氯亚铂酸铵、溴化铂、溴铂酸、碘铂、二亚硝基二氨铂、硝酸铂、四氨合硝酸铂、亚硫酸铂、甲啶铂吡铂、奈达铂、顺铂、卡铂、米铂、依铂、奥沙利铂、二腈苯基二氯化铂、三苯基膦氯化铂中的一种或多种。
Cu的金属前体为可溶性铜盐,包括:乙酸铜、氯化亚铜、溴化亚铜、碘化亚铜、氟化铜、氯化铜、溴化铜、硫酸铜、硝酸铜、甲酸铜、乙酰丙酮铜、柠檬酸铜、葡萄糖酸铜、甘氨酸铜、环烷酸铜、草酸铜、酞菁铜、四氟硼酸铜中的一种或多种。
Te的金属前体为含碲的可溶性化合物,包括:碲酸、亚碲酸、亚碲酸锂、亚碲酸钠、亚碲酸钾、亚碲酸钙、亚碲酸锶、亚碲酸钡、亚碲酸镉、亚碲酸铜、亚碲酸银、碲酸钠、原碲酸钠、原碲酸氢钠、碲酸钾、原碲酸氢钾、碲酸铵、碲酸钡、原碲酸铋、碲酸银、原碲酸汞、甲碲醇、乙碲醇、苯碲酚、2,4,6-三甲基苯碲酚、二甲基碲、二(三氟甲基)碲、二苯基二碲、碲半胱氨酸、羰基碲、四碲代硅酸铯、四碲代钒酸亚铜、五氟碲酸、六氯合碲酸钾、三苯基碲化膦、四甲醇碲、四乙醇碲中的一种或多种。
还原剂用于将相应的金属前体中的金属离子还原为金属原子,例如将Pt的金属前体还原为Pt,将Cu的金属前体还原为Cu,Te的金属前体还原为Te。还原剂包括无水柠檬酸、甲酸、甲醛、抗坏血酸、间苯三酚、葡萄糖中的一种或多种。
溶剂用于溶解Pt的金属前体、Cu的金属前体、Te的金属前体,溶剂可以为N, N-二甲基乙酰胺、水、乙二醇、苯甲醇、甲酰胺、N, N-二甲基甲酰胺、油胺、油酸、十八烯等,本公开对此不做限制。
在一个示例中,反应液中还包括助剂,助剂为羰基化合物,其中羰基会和Pt结合,调节Pt的还原速度。包括:CO气体、羰基钼、羰基钒、羰基铬、羰基锰、羰基铁、羰基钴、羰基镍、羰基锝、羰基钌、羰基铑、羰基钨、羰基铼、羰基锇、羰基铱等。
在一个示例中,反应液中还包括保护剂,保护剂用于防止纳米颗粒团聚,保护剂可以为:聚乙烯吡咯烷酮、聚烯丙基胺盐酸盐、曲拉通X-100、十六烷基三甲基氯化铵、十八烷基三甲基氯化铵、十六烷基三甲基溴化铵、十八烷基三甲基溴化胺、十二烷基三甲基氯化铵、十二烷基苯磺酸钠、十二烷基硫酸钠、双十二烷基二甲基溴化铵、环氧乙烯-苯乙烯PEO(2200)-b-PS(5000)、聚氧化乙烯-聚甲基丙烯酸甲酯PEO(10500)-b-PMMA(18000)等。
为了使溶剂中的各组分混合均匀,可以通过超声分散,以使各组分均匀分散在溶剂中,得到均质的反应液。
步骤102、将所述反应液转移至反应釜中进行水热反应,反应结束后得到PtCuTe纳米材料。
将反应液转移至聚四氟乙烯内衬的反应釜中进行水热反应,水热反应温度为140-300℃,水热反应时间为1-24h。反应结束后,将反应釜内的产物过滤、洗涤,得到PtCuTe纳米材料。
本公开实施例还提供一种修复凝胶,包括PtCuTe纳米材料、聚乙烯醇凝胶和水;其中,PtCuTe纳米材料的浓度为1-10μg/mL,聚乙烯醇凝胶的浓度为300-500 mg/mL。
下面结合具体实施例对本方案做详细说明。
实施例1
一种PtCuTe纳米材料的制备方法,包括如下步骤:
(1)分别称量10 mg 乙酰丙酮铂,3 mg 乙酸铜,12 mg 碲酸Te(OH)6,3 mg Mo(CO)6,200 mg 聚乙烯吡咯烷酮,60 mg 无水柠檬酸,分散于10 mL N, N-二甲基乙酰胺中,超声分散均匀后,得到反应液;
(2)将反应液转移到聚四氟乙烯内衬的反应釜中,200℃反应 8小时;反应结束后,过滤、洗涤,得到PtCuTe纳米材料。
一、PtCuTe纳米材料的表征
如图2a至图2h所示,为实施例1制备的PtCuTe纳米材料的表征结果,包括TEM、XRD、电子显微镜图及元素分布、元素定量分析、XPS图谱。
1、如图2a-2d为高分辨率透射电子显微镜TEM图像,结果显示PtCuTe为二维纳米材料,二维纳米材料有较高的比表面积、大量的活性位点、良好的导电性,因此在制备各种基于二维材料的功能纳米酶方面具有巨大优势。
2、X射线衍射图谱(XRD)如图2e所示,根据特征峰比对,确定成功制备出PtCuTe纳米材料。
3、高角度环形暗场射扫描投射电子显微镜图及元素分布图如图2f所示,表征成功制备出PtCuTe纳米材料。
4、ICP-AES元素定量分析如图2g所示,经过元素定量分析计算,Pt、Cu、Te三种原子比为28.5:10.8:60.7。
5、Pt 4f XPS图谱如图2h所示,根据附图可以看出71.8eV、75eV处的主峰分别对应Pt 4f7/2、Pt 4f5/2,主峰在Pt0峰与Pt2+峰之间,表明PtCuTe纳米材料中的Pt处于低氧化价态。
二、PtCuTe纳米材料的酶催化活性
1、PtCuTe纳米材料对3,3',5,5'-四甲基联苯胺(TMB)-H2O2的新型荧光指示剂反应产生强催化作用。
具体操作方法:500μL TMB(0.25 mM)和500μL H2O2(3 mM)混合均匀后,分别添加不同浓度的PtCuTe,使混合液PtCuTe终浓度为10μg/mL、20μg/mL、40μg/mL、80μg/mL,测其在625nm处的紫外吸光值。
催化效果如图3所示,根据图3可知,因PtCuTe纳米材料具有较强的类过氧化物酶催化活性,能够催化H2O2氧化TMB。进一步可以看出PtCuTe纳米材料的纳米酶催化活性呈浓度依赖性增强。
2、为了验证PtCuTe纳米材料对羟基自由基(.OH)的清除能力,具体做法:1.8mMFeSO4·7H2O和5mM H2O2的芬顿(Fenton)反应产生.OH,反应时间为10分钟。分别添加不同浓度的PtCuTe纳米材料,使混合液PtCuTe终浓度为10μg/mL、20μg/mL、40μg/mL、80μg/mL,5,5-二甲基-1-吡咯啉-N-氧化物(5,5-Dimethyl-1-pyrrolineN-oxide,DMPO)通过电子顺磁共振(EPR)自旋捕获来测量.OH。
如图4所示为PtCuTe 纳米材料清除.OH的电子顺磁共振波,实验结果表明PtCuTe纳米材料的浓度越高,其清除.OH能力越强。
图5所示为不同浓度PtCuTe 纳米材料清除.OH的效果示意图,定量分析显示PtCuTe 纳米材料清除.OH活性呈浓度依赖性增强。
三、PtCuTe纳米材料对金黄色葡萄球菌的抑制作用
具体操作方法:将1mL金黄色葡萄球菌悬浮液(1010CFU mL-1)分别加入不同浓度的PtCuTe水溶液中(0.25μg/mL,0.50μg/mL,1.00μg /mL,2.00μg /mL),在37℃、5%CO2下孵育24小时,细菌培养液中均加入了针对细菌的超氧化物歧化酶和过氧化氢酶将ROS浓度控制在较低水平。
通过细菌活体染色、稀释涂布平板计数方法分析PtCuTe纳米材料对金黄色葡萄球菌的抑制作用。如图6a为空白对照组(control)、0.25 μg/mL PtCuTe组、0.50 μg/mLPtCuTe组、1.00 μg/mL PtCuTe组、2.00 μg/mL PtCuTe组金黄色葡萄球菌稀释涂布后的菌落形态图;图6b为图6a的菌落形成单位定量分析;图6c为各组金黄色葡萄球菌活体染色;图6d为各组金黄色葡萄球菌扫描电镜图。根据图6a-6d结果显示PtCuTe纳米材料对金黄色葡萄球菌有显著的抑制生长作用,扫面电镜图显示PtCuTe纳米材料能够破坏金黄色葡萄球菌细胞壁,从而抑制其繁殖。
四、PtCuTe纳米材料可以逆转高糖环境下人脐静脉内皮细胞成血管功能的下降
具体操作方法:将人脐静脉内皮细胞分为四组,分别用正常培养基(内皮细胞培养基,Endothelial Cell Medium, ECM)(NG)、加25mM葡萄糖培养基(HG)、25mM葡萄糖+0.25 μg/mL PtCuTe(HG+0.25)、25mM葡萄糖+0.50 μg/mL PtCuTe(HG+0.50),于 37℃培养箱中培养24小时。然后24孔板里加入300μl的基质胶,在37℃培养箱中固化30分钟。固化后加入500μl 1×106个经过上述四组不同预处理的脐静脉内皮细胞,在培养箱中培养4h。
如图7a为正常组(NG)、高糖组(HG)、高糖+0.25 μg/mL PtCuTe组 (HG+0.25)、高糖+0.50 μg/mL PtCuTe 组(HG+0.50) 内皮细胞管腔形成实验图;图7b为各组内皮细胞管腔形成实验图,从左至右依次为正常组(NG)、高糖组(HG)、高糖+0.25 μg/mL PtCuTe组 (HG+0.25)、高糖+0.50 μg/mL PtCuTe 组(HG+0.50)对应的结果。根据图7a-7b结果显示PtCuTe纳米材料可以逆转高糖环境下人脐静脉内皮细胞成血管功能的下降,定量分析显示PtCuTe纳米材料可以明显促进管腔长度、分支数目和管腔数目。
五、PtCuTe纳米材料可以逆转高糖环境下人真皮成纤维细胞迁移运动功能的下降
具体操作方法:将人真皮成纤维细胞接种在24孔板中,使细胞铺满底板约50%,分别用正常培养基(内皮细胞培养基,Endothelial Cell Medium,ECM)(NG)、加25mM葡萄糖培养基(HG)、25mM葡萄糖+0.25 μg/mL PtCuTe(HG+0.25)、25mM葡萄糖+0.50 μg/mL PtCuTe(HG+0.50) ,于37℃培养箱中培养24小时。将24孔板置于活细胞成像*** (AppliedPrecision,美国)中,并在37℃和5%CO2下孵育6小时,检测各组细胞运动轨迹,细胞轨迹通过Imaris 9.7(Dell,美国)进行分析。
如图8a为正常组(NG)、高糖组(HG)、高糖+0.25 μg/mL PtCuTe组 (HG+0.25)、高糖+0.50 μg/mL PtCuTe 组(HG+0.50) 成纤维细胞运动轨迹图;图8b为各组真皮成纤维细胞运动速度;图8c为运动轨迹长度。根据图8a-8c定量分析结果表明:PtCuTe纳米材料可以逆转高糖环境下人真皮成纤维细胞迁移运动功能的下降。
六、PtCuTe纳米材料可以逆转高糖环境下人巨噬细胞向促炎型极化,促进其向抗炎型极化
具体操作方法:人单核细胞白血病细胞用50nM佛波酯(PMA)诱导分化为巨噬细胞后,巨噬细胞分为四组,分别用正常培养基(内皮细胞培养基,Endothelial Cell Medium,ECM)(NG)、加25mM葡萄糖培养基(HG)、25mM葡萄糖+0.25 μg/mL PtCuTe(HG+0.25)、25mM葡萄糖+0.50 μg/mL PtCuTe(HG+0.50),于37℃培养箱中培养24小时。分别用M1促炎型标记分子CD11c、M2抗炎型标记分子CD206进行标记,流式细胞仪检测各组CD11c、CD206的表达情况。
如图9a为正常组(NG)、高糖组(HG)、高糖+0.25 μg/mL PtCuTe组 (HG+0.25)、高糖+0.50 μg/mL PtCuTe 组(HG+0.50) 巨噬细胞极化分型流式细胞结果图;图9b和图9c为流式细胞结果,图9b为CD11c所占的比率,图9c为CD206所占的比例,图中从左至右依次为正常组(NG)、高糖组(HG)、高糖+0.25 μg/mL PtCuTe组 (HG+0.25)、高糖+0.50 μg/mL PtCuTe组(HG+0.50)对应的结果。根据图9a-9c定量分析显示:PtCuTe纳米材料可以逆转高糖环境下人巨噬细胞向促炎M1型极化,促进其向抗炎M2型极化。
实施例2
一种修复凝胶,包括实施例1制备的PtCuTe纳米材料,聚乙烯醇凝胶和去离子水。该修复凝胶的制备方法为:
将实施例1制备的PtCuTe纳米材料分散在去离子水中,使得PtCuTe纳米材料的浓度为5ug/ml,再加入聚乙烯醇凝胶,聚乙烯醇凝胶浓度为300mg/mL。
以15只小鼠作为本次实验对象,将15只小鼠背部剃毛后,在每只小鼠的背部制作直径为6mm的全层皮肤伤口。随后,将100μL金黄色葡萄球菌液(1×106)接种到各个小鼠的伤口上。将15只小鼠随机分为三组(每组5只),其中一组为对照小鼠,另外两组为糖尿病小鼠。NG组为用300mg/mL的聚乙烯醇凝胶涂覆对照小鼠的伤口;HG组为用300mg/mL聚乙烯醇凝胶涂抹糖尿病小鼠组的伤口;HG+ PtCuTe组为实施例2制备的修复凝胶(300mg/mLPVA+5.0μg/mLPtCuTe)涂抹糖尿病小鼠的伤口。在第1、3、5天, 分别用以上不同凝胶处理伤口,在第0、2、4、6、8天,拍摄各组伤口照片,通过Image J软件对伤口进行测量和分析。
如图10a为NG组、HG组、HG+ 5.0 μg/mL PtCuTe组小鼠皮肤缺损局部第0、8天形态图及愈合比例模式图;图10b位各组皮肤愈合百分率折线图。图10a-10b结果表明:PtCuTe纳米材料可以有效促进糖尿病小鼠皮肤伤口愈合,(显著性P<0.001)。
实施例3
一种PtCuTe纳米材料的制备方法,包括如下步骤:
(1)分别称量10 mg氯铂酸,3 mg 氯化铜,12 mg 亚碲酸,60 mg 抗坏血酸,分散于10 mL N, N-二甲基乙酰胺中,超声分散均匀后,得到反应液;
(2)将反应液转移到聚四氟乙烯内衬的反应釜中,140℃反应24小时;反应结束后,过滤、洗涤,得到PtCuTe纳米材料。
实施例4
一种PtCuTe纳米材料的制备方法,包括如下步骤:
(1)分别称量10 mg乙二胺氯化铂,3 mg草酸铜,12 mg 三苯基碲化膦,60 mg 甲酸,200 mg十八烷基三甲基氯化铵、3 mg羰基钒分散于10 mL N, N-二甲基甲酰胺中,超声分散均匀后,得到反应液;
(2)将反应液转移到聚四氟乙烯内衬的反应釜中,300℃反应2小时;反应结束后,过滤、洗涤,得到PtCuTe纳米材料。
实施例5
一种PtCuTe纳米材料的制备方法,包括如下步骤:
(1)分别称量10 mg乙酰丙酮铂,3 mg 乙酰丙酮铜,12 mg 亚碲酸,60 mg 抗坏血酸,200 mg十六烷基三甲基氯化铵,3 mg羰基钴分散于10 mL N, N-二甲基乙酰胺中,超声分散均匀后,得到反应液;
(2)将反应液转移到聚四氟乙烯内衬的反应釜中,220℃反应6小时;反应结束后,过滤、洗涤,得到PtCuTe纳米材料。
实施例6
一种PtCuTe纳米材料的制备方法,包括如下步骤:
(1)分别称量5 mg氯铂酸、5 mg三苯基膦氯化铂,1 mg 氯化铜,2 mg柠檬酸铜,6mg 亚碲酸,6mg甲碲醇,60 mg 抗坏血酸,200 mg聚乙烯吡咯烷酮,3mg羰基钼分散于10 mLN, N-二甲基甲酰胺中,超声分散均匀后,得到反应液;
(2)将反应液转移到聚四氟乙烯内衬的反应釜中,180℃反应15小时;反应结束后,过滤、洗涤,得到PtCuTe纳米材料。
应该理解,可以使用上面所示的各种形式的流程,重新排序、增加或删除步骤。例如,本发公开中记载的各步骤可以并行地执行也可以顺序地执行也可以不同的次序执行,只要能够实现本公开公开的技术方案所期望的结果,本文在此不进行限制。
此外,术语“第一”、“第二”仅用于描述目的,而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。由此,限定有“第一”、“第二”的特征可以明示或隐含地包括至少一个该特征。在本公开的描述中,“多个”的含义是两个或两个以上,除非另有明确具体的限定。
以上所述,仅为本公开的具体实施方式,但本公开的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本公开揭露的技术范围内,可轻易想到变化或替换,都应涵盖在本公开的保护范围之内。因此,本公开的保护范围应以所述权利要求的保护范围为准。
Claims (8)
1.一种PtCuTe纳米材料的制备方法,其特征在于,所述方法包括:
将可溶性Pt盐、可溶性Cu盐、含Te的可溶性化合物、还原剂及保护剂均匀分散在溶剂中,得到反应液;
将所述反应液转移至反应釜中进行水热反应,所述水热反应的条件为:水热温度140-300℃,水热时间1-24h,反应结束后得到PtCuTe纳米材料;其中所述保护剂用于防止水热反应过程生成的纳米颗粒体团聚。
2.根据权利要求1所述的方法,其特征在于,所述反应液中还包括助剂,所述助剂用于调节还原速度。
3.根据权利要求1所述的方法,其特征在于,所述可溶性Pt盐包括:乙酰丙酮铂、氯铂酸、氯铂酸钾、氯铂酸铵、四氯合铂四氨合铂酸盐、氯铂酸钠、氯化铂、乙二胺氯化铂、氯亚铂酸、氯亚铂酸钾、氯亚铂酸铵、溴化铂、溴铂酸、碘铂、二亚硝基二氨铂、硝酸铂、四氨合硝酸铂、亚硫酸铂、甲啶铂吡铂、奈达铂、顺铂、卡铂、米铂、依铂、奥沙利铂、二腈苯基二氯化铂、三苯基膦氯化铂中的一种或多种。
4.根据权利要求1所述的方法,其特征在于,所述可溶性Cu盐包括:乙酸铜、氯化亚铜、溴化亚铜、碘化亚铜、氟化铜、氯化铜、溴化铜、硫酸铜、硝酸铜、甲酸铜、乙酰丙酮铜、柠檬酸铜、葡萄糖酸铜、甘氨酸铜、环烷酸铜、草酸铜、酞菁铜、四氟硼酸铜中的一种或多种。
5.根据权利要求1所述的方法,其特征在于,所述含Te的可溶性化合物包括:碲酸、亚碲酸、亚碲酸锂、亚碲酸钠、亚碲酸钾、亚碲酸钙、亚碲酸锶、亚碲酸钡、亚碲酸镉、亚碲酸铜、亚碲酸银、碲酸钠、原碲酸钠、原碲酸氢钠、碲酸钾、原碲酸氢钾、碲酸铵、碲酸钡、原碲酸铋、碲酸银、原碲酸汞、甲碲醇、乙碲醇、苯碲酚、2,4,6-三甲基苯碲酚、二甲基碲、二(三氟甲基)碲、二苯基二碲、碲半胱氨酸、羰基碲、四碲代硅酸铯、四碲代钒酸亚铜、五氟碲酸、六氯合碲酸钾、三苯基碲化膦、四甲醇碲、四乙醇碲中的一种或多种。
6.根据权利要求2所述的方法,其特征在于,所述助剂为羰基化合物。
7.一种PtCuTe纳米材料,其特征在于,根据权利要求1-6任一项所述方法制备。
8.一种修复凝胶,其特征在于,包括权利要求7所述的PtCuTe纳米材料、聚乙烯醇凝胶和水,所述PtCuTe纳米材料的浓度为1-10μg/mL,所述聚乙烯醇凝胶浓度为300-500 mg/mL。
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