CN108927528A - 一种以木耳多糖为模板制备纳米铂粒子的方法 - Google Patents
一种以木耳多糖为模板制备纳米铂粒子的方法 Download PDFInfo
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002245 particle Substances 0.000 title claims abstract description 30
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 29
- 150000004676 glycans Chemical class 0.000 title claims abstract description 24
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 24
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 17
- 241000221377 Auricularia Species 0.000 title claims 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011591 potassium Substances 0.000 claims abstract description 8
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims 1
- 241000233866 Fungi Species 0.000 abstract description 25
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 20
- 238000002835 absorbance Methods 0.000 description 9
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 7
- 102000003992 Peroxidases Human genes 0.000 description 7
- 239000008103 glucose Substances 0.000 description 7
- 108040007629 peroxidase activity proteins Proteins 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- 102000004190 Enzymes Human genes 0.000 description 4
- 108090000790 Enzymes Proteins 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229940088598 enzyme Drugs 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000002082 metal nanoparticle Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 238000004627 transmission electron microscopy Methods 0.000 description 3
- 108010015776 Glucose oxidase Proteins 0.000 description 2
- 239000004366 Glucose oxidase Substances 0.000 description 2
- 239000007853 buffer solution Substances 0.000 description 2
- 229940116332 glucose oxidase Drugs 0.000 description 2
- 235000019420 glucose oxidase Nutrition 0.000 description 2
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- 102000007562 Serum Albumin Human genes 0.000 description 1
- 108010071390 Serum Albumin Proteins 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000011942 biocatalyst Substances 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000003278 mimic effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000005502 peroxidation Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007974 sodium acetate buffer Substances 0.000 description 1
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
一种以木耳多糖为模板制备纳米铂粒子的方法,其主要是按蒸馏水与木耳多糖质量比为1:1的比例,配制浓度为1mg/mL的木耳多糖溶液,按木耳多糖溶液与四氯铂酸钾溶液的摩尔比为1:300~600的比例混合均匀,将其放入金属浴中,300~500rpm,40℃~55℃下反应3h,溶液从无色慢慢变为深灰色,从而得到纳米铂粒子。本发明具有反应条件温和、操作简单、原料环保和分散稳定性好等优点。
Description
技术领域
本发明属于金属材料技术领域,特别涉及一种纳米材料的制备方法。
背景技术
酶是一种天然的生物催化剂,具有良好的催化效率和选择性。然而,天然酶具有成本高、易失活等缺点,这限制了其在许多方面的应用。贵金属纳米粒子作为一种重要的纳米材料,能够模拟过氧化物酶的催化活性,被广泛应用于各种检测。研究结果表明,贵金属纳米粒子的粒径越小,比表面积越大,活性位点越多,催化活性越大。因此,制备粒径小的贵金属纳米粒子以模拟过氧化物酶的催化活性,具有良好的应用前景。
目前,模板法是一种非常重要的制备纳米铂粒子的方法。模板法的特点是无论是在液相或气相中发生的化学反应,都能在模板的有效区域内进行,因此,能够调控纳米铂粒子的粒径和形貌,防止纳米铂粒子团聚。根据限阈能力的不同,模板法分为硬模板法和软模板法。硬模板法具有结构较为单一,所制备的纳米粒子形貌变化较少的缺点;软模板法具有操作方法简单的优点,软模板法通常采用高分子物质为模板,常用的溶菌酶、胰蛋白酶和牛血清白蛋白等蛋白质分子虽能够制备单分散的纳米铂粒子,但是此方法具有原料价格高的缺点,而且聚乙烯亚胺等高分子不能够自然降解,并有毒性。因此,还需要进一步开发新的制备纳米铂粒子的软模板。
发明内容
本发明的目的在于提供一种制备条件温和、操作容易、原料环保的以木耳多糖为模板制备纳米铂粒子的方法。本发明主要是首先配制木耳多糖溶液,利用木耳多糖的还原性还原金属铂前驱体,得到粒径均匀的纳米铂粒子。
本发明的技术方案如下:
(1)按蒸馏水与木耳多糖的质量比为1:1的比例,配制成浓度为1mg/mL的木耳多糖溶液;
(2)按木耳多糖溶液与四氯铂酸钾溶液的摩尔比为1:300~600的比例混合均匀,将其放入金属浴中,300~500rpm,40~55℃下反应3h,溶液从无色慢慢变为深灰色,从而得到纳米铂粒子。
本发明与现有技术相比具有如下优点:
1、制备工艺简单,成本低廉,反应条件温和。
2、所制得的铂纳米粒子的形貌规则、粒径均匀,稳定性好。
3、所选的模板本身具有很高的生物相容性,产品可用于生物医学领域。
附图说明
图1为本发明实施例1获得的木耳多糖-铂纳米粒子的TEM图。
图2为本发明实例1模拟过氧化物酶最佳温度图。
图3为本发明实例1模拟过氧化物酶最佳pH图。
图4为本发明实例1应用于检测不同浓度的葡萄糖吸光度与浓度间线性图。
图5为本发明实施例2获得的木耳多糖-铂纳米粒子的TEM图。
图6为本发明实施例3获得的木耳多糖-铂纳米粒子的TEM图。
具体实施方式
实施例1
取木耳多糖溶于蒸馏水中,配制成浓度为1mg/mL的木耳多糖溶液,将木耳多糖溶液与四氯铂酸钾溶液按1:300的比例混合后放入金属浴中,控制转速为500rpm,温度为40℃条件下反应3h,溶液从无色缓慢变成深灰色,即获得木耳多糖-纳米铂粒子。
应用透射电子显微镜对纳米铂粒字进行形貌表征,如图1所示,纳米铂粒子的直径为0.99nm左右,形貌规则,呈球状。
为研究纳米铂粒子模拟过氧化物酶的催化活性,设置如下实验:
1)取实施例1样品50μL,加入相同pH的缓冲溶液1000μL;用金属浴在不同温度下保温10min,向其中加入TMB 300μL,保温10min;4)加入H2O250μL(0.03M),设定温度下反应10min;之后在紫外下测量吸光度,观察在652nm波长处的吸光度值,得到吸光度随T的变化曲线,如图2所示。
2)取实施例1样品50μL,加入不同pH的缓冲溶液1000μL;用金属浴在相同温度下保温10min,向其中加入TMB 300μL,保温10min;4)加入H2O250μL(0.03M),设定温度下反应10min;之后在紫外下测量吸光度,观察在652nm波长处的吸光度值,得到吸光度随pH的变化曲线,如图3所示。
通过该实验得出纳米铂粒子模拟过氧化物酶的最佳条件。
为研究纳米铂粒子模拟过氧化物酶能否应用于检测葡萄糖浓度,设置如下实验:
取葡萄糖氧化酶(GOx)100μL,分别加入不同浓度(0.04mM-1mM)的葡萄糖200μL于2mL离心管,金属浴50℃下加热30min;另取实施例1样品200μL于另一离心管中,加入pH=4的醋酸-醋酸钠缓冲液300μL,再加入700μL TMB溶液,金属浴最适温度25℃下加热15min;将上述的TMB溶液分别加入到每个葡萄糖溶液中,金属浴25℃下反应30min;
应用紫外在652nm下测量吸光度,如图4所示,葡萄糖浓度在0.04-1mM之间时,吸光度与浓度间呈良好线性关系(y=0.45803x+0.05257),因此说明利用该纳米粒子模拟过氧化物酶检测葡萄糖的方法灵敏度较高。
实施例2
取木耳多糖溶于蒸馏水中,配制成浓度为1mg/mL的木耳多糖溶液,将木耳多糖溶液与四氯铂酸钾溶液按1:500的比例混合后放入金属浴中,控制转速为400rpm,温度为50℃条件下反应3h,溶液从无色缓慢变成深灰色,即获得木耳多糖-纳米铂粒子。
应用透射电子显微镜对纳米铂粒子进行形貌表征,如图5所示,纳米铂粒子的直径为1.19nm左右,形貌规则,呈球状。
实施例3
取木耳多糖溶于蒸馏水中,配制成浓度为1mg/mL的木耳多糖溶液,将木耳多糖溶液与四氯铂酸钾溶液按1:600的比例混合后放入金属浴中,控制转速为300rpm,温度为55℃条件下反应3h,溶液从无色缓慢变成深灰色,即获得木耳多糖-纳米铂粒子。
应用透射电子显微镜对纳米铂粒子进行形貌表征,如图6所示,纳米铂粒子的直径为1.58nm左右,形貌规则,呈球状。
Claims (1)
1.一种以木耳多糖为模板制备纳米铂粒子的方法,其特征在于:
(1)按蒸馏水与木耳多糖质量比为1:1的比例,配制浓度为1mg/mL的木耳多糖溶液;
(2)按木耳多糖和四氯铂酸钾溶液的摩尔比为1:300~600的比例,将步骤(1)的木耳多糖溶液和四氯铂酸钾溶液混合均匀,放入金属浴中,300~500rpm,40~55℃下反应3h,溶液从无色慢慢变为深灰色,从而得到纳米铂粒子。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009044146A1 (en) * | 2007-10-02 | 2009-04-09 | University Of York | Metal nanoparticles |
| WO2010010123A1 (en) * | 2008-07-23 | 2010-01-28 | Universita' Degli Studi Di Trieste | Three-dimensional nanocomposite materials consisting of a polysaccharidic matrix and metallic nanoparticles, preparation and use thereof |
| CN101733411A (zh) * | 2009-12-15 | 2010-06-16 | 武汉大学 | 一种生物相容的铂纳米颗粒的制备方法 |
| CN107486562A (zh) * | 2017-11-09 | 2017-12-19 | 西北师范大学 | 植物源性多糖提取物还原金属盐制备金属纳米材料的方法及应用 |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009044146A1 (en) * | 2007-10-02 | 2009-04-09 | University Of York | Metal nanoparticles |
| WO2010010123A1 (en) * | 2008-07-23 | 2010-01-28 | Universita' Degli Studi Di Trieste | Three-dimensional nanocomposite materials consisting of a polysaccharidic matrix and metallic nanoparticles, preparation and use thereof |
| CN101733411A (zh) * | 2009-12-15 | 2010-06-16 | 武汉大学 | 一种生物相容的铂纳米颗粒的制备方法 |
| CN107486562A (zh) * | 2017-11-09 | 2017-12-19 | 西北师范大学 | 植物源性多糖提取物还原金属盐制备金属纳米材料的方法及应用 |
Non-Patent Citations (2)
| Title |
|---|
| 邓兰青等: "多糖模板调控纳米无机晶体生长", 《人工晶体学报》 * |
| 郑晓凤等: "桔梗多糖软模板法制备纳米硒的抗氧化及抗肿瘤活性研究", 《微量元素与健康研究》 * |
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Application publication date: 20181204 |