CN110398526A - 一种金-海芋杆基多孔碳复合材料修饰电极的制备与芦丁的检测应用 - Google Patents
一种金-海芋杆基多孔碳复合材料修饰电极的制备与芦丁的检测应用 Download PDFInfo
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Abstract
通过溶剂热法合成金微球负载海芋基多孔碳复合物(Au@APC),将适量的Au@APC分散液直接滴涂在基底电极—碳离子液体电极(CILE)表面得到Au@APC/CILE。利用扫描电镜和透射电镜对APC和Au@APC的结构与表面形貌进行了分析。通过循环伏安法探究了芦丁在Au@APC/CILE上的电化学行为。利用差分脉冲伏安法(DPV)探究了不同浓度的芦丁和对应氧化峰电流的线性关系,得到检测范围为0.12‑10.0μmol L‑1,检测限0.0265μmol L‑1。
Description
技术领域
本发明涉及纳米材料的制备与化学修饰电极的电化学传感技术领域,具体涉及到一种金(Au)负载海芋杆基多孔碳(APC)修饰电极的制备方法和检测芦丁含量的方法。
背景技术
采用生物质制备活性炭的研究在近年来发展迅速,所采用的制备方法主要有催化活化法、直接碳化法和水热碳化法等。利用热带地区常见的植物海芋的杆做为原料和生物质前驱体热解碳化制备的多孔碳材料,具有高比表面积、高稳定性、价格便宜,可应用于能量储存和工业催化等领域,尤其在环境保护和海洋资源有效利用方面意义重大。
芦丁(Rutin)是具有多种生物活性的黄酮类化合物,广泛存在于植物界,在我国储量丰富,早已用于工业化生产。随着现代药物化学及现代制剂技术的发展,芦丁的研究呈现生机勃勃的前景,一些新的药理作用的发现(如抗前列腺癌,结肠癌,肝癌等)以及新的提取纯化工艺(如超临界二氧化碳萃取技术)的应用使得芦丁的提取纯化更加绿色、环保。但定性或定量检测药物或植物中芦丁的含量,比如高效液相色谱法(HPLC)、毛细管电泳(CE)等,具有仪器昂贵,操作复杂,耗时,而用电化学方法检测芦丁具有方便,响应快,灵敏度高,检测范围高,造价低等优点。
发明内容
一种金(Au)负载海芋杆基多孔碳(APC)复合材料的制备和应用,其特征在于碳离子液体的电极表面修饰APC和Au的方法,测试所述修饰电极电化学行为的方法,其特征在于,包括以下步骤:
(1) APC的制备
将海芋杆在2.0 mol L-1 KOH中浸泡12 h,过滤后在90℃条件下干燥1 h,干燥的后的海芋杆放置在管式炉中热解。其次,将得到黑色固体在3.0 mol L-1 HCl中浸泡1 h,然后用蒸馏水反复清洗至中性。最后,将产物放置在烘箱中120 ℃脱水6 h;
(2) Au/APC复合材料的制备
将步骤(1)所制得的APC分散于水中制备分散液,准确称量一定量APC分散液与H4AuCl和乙二醇混合,然后转移到50 mL聚四氟乙烯高压反应釜中反应1 h。用蒸馏水洗涤去除溶解杂质,然后在120℃干燥6 h,保存备用并命名为Au@APC;
(3) Au/APC复合材料浓度的优化
配制Au@APC复合材料分散液浓度为0.5、1.0、1.5、2.0 mg mL-1,准确量取6 μL滴涂在碳离子液体电极(CILE)表面,干燥2 h。在0.1 mmol L-1 [Fe(CN)6]3-/4-和0.1 mol L-1 KCl混合液中对四种修饰电极分别进行循环伏安扫描测定,分析所得实验结果可知修饰在CILE表面Au@APC的最佳浓度;
(4) 再取优化后的Au@APC溶液滴涂在CILE电极表面,在室温下自然晾干即可得到Au@APC/CILE电极。
根据权利书要求1所述的制备方法,其特征在于,所述(1)步骤中管式炉在600 ℃热解3 h。
如权利书要求1所述的制备方法,其特征在于,所述(2)步骤中,APC的浓度为10 mgml-1,H4AuCl溶液浓度为6 mmol L-1。
如权利书要求1所述的制备方法,其特征在于,所述(3)步骤中Au/APC最优浓度为1.5 mg mL-1。
如权利书要求1~4任一项所述的金(Au)负载海芋杆基多孔碳(APC)修饰电极步可用于实际样品中芦丁含量的分析应用。
权利要求5所述的金(Au)负载海芋杆基多孔碳(APC)修饰电极的检测环境为在pH3.0的磷酸盐缓冲溶液中。
附图说明
图1 为Au@APC不同放大倍率下的SEM图;
图2 1.0×10-4 mol L-1的芦丁在(A) Au@APC/CILE和(B) CILE上的循环伏安曲线;
图3 不同pH下1.0×10-4 mol L-1芦丁在Au@APC/CILE上的循环伏安叠加图(从a到j: 2.0, 3.0, 4.0, 5.0, 6.0, 7.0, 8.0),扫速为100 mV/s;
图4 不同扫速下1.0×10-4 mol L-1芦丁在Au@APC/CILE上的循环伏安叠加图(从a到l: 0.05, 0.1, 0.15, 0.2, 0.25, 0.3, 0.35, 0.4, 0.45, 0.5, 0.55, 0.6 Vs-1);
图5 不同浓度芦丁在Au@APC/CILE上的DPV曲线叠加图(A) (从a到m: 0.12,0.24, 0.96, 1.2, 1.4, 1.6, 1.8, 2.0, 4.0, 6.0, 8.0, 10.0 μmol L-1),其中插图为氧化峰电流与芦丁的浓度之间的关系曲线图。
Claims (6)
1.一种金(Au)负载海芋杆基多孔碳(APC)复合材料的制备和应用,其特征在于碳离子液体的电极表面修饰APC和Au的方法,测试所述修饰电极电化学行为的方法,其特征在于,包括以下步骤:
(1) APC的制备
将海芋杆在2.0 mol L-1 KOH中浸泡12 h,过滤后在90℃条件下干燥1 h,干燥的后的海芋杆放置在管式炉中热解,其次,将得到黑色固体在3.0 mol L-1 HCl中浸泡1 h,然后用蒸馏水反复清洗至中性,最后,将产物放置在烘箱中120 ℃脱水6 h;
(2) Au/APC复合材料的制备
将步骤(1)所制得的APC分散于水中制备分散液,准确称量一定量APC分散液与H4AuCl和乙二醇混合,然后转移到50 mL聚四氟乙烯高压反应釜中反应1 h,
用蒸馏水洗涤去除溶解杂质,然后在120℃干燥6 h,保存备用并命名为Au@APC;
(3) Au/APC复合材料浓度的优化
配制Au@APC复合材料分散液浓度为0.5、1.0、1.5、2.0 mg mL-1,准确量取6 μL滴涂在碳离子液体电极(CILE)表面,干燥2 h,
在0.1 mmol L-1 [Fe(CN)6]3-/4-和0.1 mol L-1 KCl混合液中对四种修饰电极分别进行循环伏安扫描测定,分析所得实验结果可知修饰在CILE表面Au@APC的最佳浓度;
(4) 再取优化后的Au@APC溶液滴涂在CILE电极表面,在室温下自然晾干即可得到Au@APC/CILE电极。
2.根据权利书要求1所述的制备方法,其特征在于,所述(1)步骤中管式炉在600 ℃热解3 h。
3.如权利书要求1所述的制备方法,其特征在于,所述(2)步骤中,APC的浓度为10 mgml-1,H4AuCl溶液浓度为6 mmol L-1。
4.如权利书要求1所述的制备方法,其特征在于,所述(3)步骤中Au/APC最优浓度为1.5mg mL-1。
5.如权利书要求1~4任一项所述的金(Au)负载海芋杆基多孔碳(APC)修饰电极步可用于实际样品中芦丁含量的分析应用。
6.权利要求5所述的金(Au)负载海芋杆基多孔碳(APC)修饰电极的检测环境为在pH3.0的磷酸盐缓冲溶液中。
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CN113433180A (zh) * | 2021-05-12 | 2021-09-24 | 江西农业大学 | 一种对芦丁检测的电化学传感方法 |
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