CN110646479A - 一种比率电化学传感器用于检测对乙酰氨基苯酚 - Google Patents
一种比率电化学传感器用于检测对乙酰氨基苯酚 Download PDFInfo
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Abstract
本发明公开了一种基于二茂铁‑氧化石墨烯复合物修饰的玻碳电极构建的电化学传感器,用于高效检测对乙酰氨基苯酚(4‑AC)。首先,通过超声的方法制备二茂铁‑氧化石墨烯复合物悬浊液,然后加入一定量萘芬溶液,形成二茂铁‑氧化石墨烯复合物溶液。然后将上述溶液滴涂于玻碳电极表面将其作为工作电极,Ag/AgCl电极作为参比电极,以Pt丝电极为辅助电极。其中,二茂铁在电化学驱动力作用下产生的氧化还原峰作为电极表面的参比信号,然后以含有不同浓度的、4‑AC的磷酸盐缓冲溶液(PBS)为电解液进行电化学检测,乙酰氨基苯酚与二茂铁峰电流的比作为最后结果从而构成了比率传感器,可以消除背景峰电流的干扰和检测仪器自身带来的系统误差。
Description
技术领域
本发明属于电化学传感器研究领域,具体涉及一种比率电化学传感器用于检测对乙酰氨基苯酚的制备方法。
背景技术
作为常用的解热镇痛药,对乙酰氨基苯酚已被广泛使用,用作缓解发烧和疼痛的有效药物。虽然乙酰氨基苯酚是相对的安全的药物,但是过量的乙酰氨基苯酚可能导致致命的肝毒性和肾毒性。因此,准确检测药物样品中的乙酰氨基苯酚的含量有助于药品质量控制,避免含量过量对人体健康构成严重危害。对于乙酰氨基苯酚的分析检测方法很多,例如分光光度法,荧光光度法,化学发光,色谱,电泳等。这些方法存在着成本高,操作复杂,灵敏性差等缺点。相比之下,电化学检测方法具有操作简单、费用低、性能好、灵敏度高、低成本的仪器、小仪器尺寸、简单操作和现场监测的优点,使其成为药物分析较好的选择。
关于化学/生物传感系统,准确的信号强度响应是十分重要的因素。由于存在很多会干扰电化学传感器识别检测信号分子的内在和外在影响因素,如传感材料含量、检测仪器工作效率和检测环境条件等。因此,单电化学信号输出模式可能会带来检测稳定性差,重复性和可靠性低等问题,使其实际应用收到了很大的限制。为了克服这些缺点,我们在此提出了一个双信号输出模式。在生物传感系统中引入一个附加信号源作为参比信号,将检测目标信号与参比信号进行求比值,作为目标信号的检测值。这样就可以降低干扰因素对检测信号的影响,从而达到精准检测目标物质浓度的目的。
发明内容
本发明公开了一种比率电化学传感器用于检测对乙酰氨基苯酚的制备方法,其中二茂铁-氧化石墨烯复合物为修饰物附着在电极表面,用于提高电极的催化性能,而且二茂铁作为参比信号源,可以得到目标检测信号的比率值,降低干扰因素对于检测结果的影响。二茂铁-氧化石墨烯复合物修饰电极构建的生物传感体系,达到高灵敏、低成本、高稳定的比率检测乙酰氨基苯酚的目标。
1. 本发明通过下述方案实现:一种比率电化学传感器用于检测对乙酰氨基苯酚的制备方法,其特征在于包括如下步骤:
(1)首先将一定量的二茂铁与氧化石墨烯溶液混合,超声30分钟。
(2)将(1)中的溶液置于离心机中,离心3~4次,直到洗至溶液无色为止,最后将上述复合物置于一定温度条件下干燥,得到纯净二茂铁-氧化石墨烯复合物。
(3)将(2)中制备的复合物分散于二次水中,配制成一定浓度的二茂铁-氧化石墨烯溶液,加入一定量萘芬溶液,制得一定浓度的二茂铁-氧化石墨烯复合物悬浮液。
(4)将玻碳电极置于含有纳米氧化铝粉末的麂皮上抛光至呈镜面,然后在乙醇溶液中超声20~30秒,再将其置于二次水中超20~30秒,最后用氮气将其吹干,获得预处理好的裸玻碳电极。
(5)取一定量(3)中制备悬浮液滴涂于预处理好的裸玻碳电极表面,直到干燥,便得到二茂铁-氧化石墨烯复合物修饰的工作电极,并将二茂铁-氧化石墨烯复合物修饰的工作电极置于含有不同浓度对乙酰氨基苯酚的磷酸盐缓冲溶液中进行电化学检测。
2. 步骤(1)一定量的二茂铁的用量为3~4mg/ml。
3. 步骤(1)中所用的氧化石墨烯的量为5mg/ml。
4. 步骤(2)中所述的烘干复合物的所需的温度为50~70℃。
5. 步骤(3)中所述的加入一定量萘芬溶液,萘芬的用量为200μL/ml, 目的是使形成的二茂铁-氧化石墨烯复合物结合稳定,使其滴涂在裸玻碳电极表面稳定,不易掉落。
6.步骤(3)中所述的一定温度条件下,其温度为70~100℃。
7.步骤(4)中所述的一定量萘芬溶液,目的是使形成的MnO2-MWCNTs复合物结合稳定,使其滴涂在金纳米颗粒聚酰亚胺聚合物膜表面稳定,不易掉落。
8. 步骤(3)中所述的制得一定浓度的二茂铁-氧化石墨烯复合物悬浮液,一定浓度为2mg/ml。
9. 步骤(5)中所述的取一定量(3)中制备悬浮液滴涂于预处理好的裸玻碳电极表面,一定量为3~5μL。
10. 步骤(5)中所述磷酸盐缓冲溶液的pH为7.4。
11. 步骤(5)中所用到的磷酸盐缓冲溶液,其浓度为5mM。
具体实施方式
以下结合附图与实施例对本发明作进一步详细描述,需要指出的是,以下所述实施例旨在便于对本发明的理解,而对其不起任何限定作用。
图1中二茂铁-氧化石墨烯复合物修饰电极用来检测磷酸钠缓冲溶液(pH 7.4)中不同浓度的4-AC的循环伏安曲线
实施例1:首先将60mg二茂铁加入20ml, 5mg/ml的氧化石墨烯溶液混合,超声30分钟。将上述步骤制得的复合物溶液置于离心机中,离心3~4次,直到洗至溶液无色为止,最后将上述复合物置于50℃条件下干燥,得到纯净二茂铁-氧化石墨烯复合物。将二茂铁-氧化石墨烯复合物分散于二次水中,配制成2mg/ml的二茂铁-氧化石墨烯复合物溶液,加入400μL萘芬溶液,制得2mg/ml的二茂铁-氧化石墨烯复合物悬浮液。将玻碳电极置于含有纳米氧化铝粉末的麂皮上抛光至呈镜面,然后在乙醇溶液中超声20秒,再将其置于二次水中超声20秒,最后用氮气将其吹干,获得预处理好的裸玻碳电极;取3μL二茂铁-氧化石墨烯复合物悬浮液涂于预处理好的裸玻碳电极表面,直到干燥,便得到二茂铁-氧化石墨烯复合物修饰的工作电极。将二茂铁-氧化石墨烯复合物修饰的工作电极置于含有不同浓度对乙酰氨基苯酚的5mM磷酸盐缓冲溶液 (pH 7.4) 中进行电化学检测。
实施例2:首先将40mg二茂铁加入10ml, 5mg/ml的氧化石墨烯溶液混合,超声30分钟。将上述步骤制得的复合物溶液置于离心机中,离心3~4次,直到洗至溶液无色为止,最后将上述复合物置于60℃条件下干燥,得到纯净二茂铁-氧化石墨烯复合物。将二茂铁-氧化石墨烯复合物分散于二次水中,配制成3mg/ml的二茂铁-氧化石墨烯复合物溶液,加入600μL萘芬溶液,制得3mg/ml的二茂铁-氧化石墨烯复合物悬浮液。将玻碳电极置于含有纳米氧化铝粉末的麂皮上抛光至呈镜面,然后在乙醇溶液中超声25秒,再将其置于二次水中超声25秒,最后用氮气将其吹干,获得预处理好的裸玻碳电极;取4μL二茂铁-氧化石墨烯复合物悬浮液涂于预处理好的裸玻碳电极表面,直到干燥,便得到二茂铁-氧化石墨烯复合物修饰的工作电极。将二茂铁-氧化石墨烯复合物修饰的工作电极置于含有不同浓度对乙酰氨基苯酚的5mM磷酸盐缓冲溶液 (pH 7.4) 中进行电化学检测。
实施例3:首先将45mg二茂铁加入25ml, 5mg/ml的氧化石墨烯溶液混合,超声30分钟。将上述步骤制得的复合物溶液置于离心机中,离心3~4次,直到洗至溶液无色为止,最后将上述复合物置于70℃条件下干燥,得到纯净二茂铁-氧化石墨烯复合物。将二茂铁-氧化石墨烯复合物分散于二次水中,配制成4mg/ml的二茂铁-氧化石墨烯复合物溶液,加入800μL萘芬溶液,制得4mg/ml的二茂铁-氧化石墨烯复合物悬浮液。将玻碳电极置于含有纳米氧化铝粉末的麂皮上抛光至呈镜面,然后在乙醇溶液中超声30秒,再将其置于二次水中超声30秒,最后用氮气将其吹干,获得预处理好的裸玻碳电极;取5μL二茂铁-氧化石墨烯复合物悬浮液涂于预处理好的裸玻碳电极表面,直到干燥,便得到二茂铁-氧化石墨烯复合物修饰的工作电极。将二茂铁-氧化石墨烯复合物修饰的工作电极置于含有不同浓度对乙酰氨基苯酚的5mM磷酸盐缓冲溶液 (pH 7.4) 中进行电化学检测。
附图说明
图1是电极循环伏案扫描曲线图。
Claims (5)
1.一种比率电化学传感器用于检测对乙酰氨基苯酚,其特征在于该方法包括如下合成步骤:
(1)首先将一定量的二茂铁与氧化石墨烯溶液混合,超声30分钟。
(2)将(1)中的溶液置于离心机中,离心3~4次,直到洗至溶液无色为止,最后将上述复合物置于一定温度条件下干燥,得到纯净二茂铁-氧化石墨烯复合物。
(3)将(2)中制备的复合物分散于二次水中,配制成一定浓度的二茂铁-氧化石墨烯溶液,加入一定量萘芬溶液,制得一定浓度的二茂铁-氧化石墨烯复合物悬浮液。
(4)将玻碳电极置于含有纳米氧化铝粉末的麂皮上抛光至呈镜面,然后在乙醇溶液中超声20~30秒,再将其置于二次水中超声20~30秒,最后用氮气将其吹干,获得预处理好的裸玻碳电极。
(5)取一定量(3)中制备悬浮液滴涂于预处理好的裸玻碳电极表面,直到干燥,便得到二茂铁-氧化石墨烯复合物修饰的工作电极,并将二茂铁-氧化石墨烯复合物修饰的工作电极置于含有不同浓度对乙酰氨基苯酚的磷酸盐缓冲溶液中进行电化学检测。
2.如权利要求1所述一种比率电化学传感器用于检测对乙酰氨基苯酚的制备方法,其特征在于,步骤(1)一定量的二茂铁的用量为3~4mg/ml,所用的氧化石墨烯的量为5mg/ml。
3.如权利要求1所述一种比率电化学传感器用于检测对乙酰氨基苯酚的制备方法,其特征在于,步骤(2)中所述的一定温度为50~70℃。
4.如权利要求1所述一种比率电化学传感器用于检测对乙酰氨基苯酚的制备方法,其特征在于,步骤(3)中所述的加入一定量萘芬溶液,萘芬的用量为200μL/ml,目的是使形成的二茂铁-氧化石墨烯复合物结合稳定,使其滴涂在裸玻碳电极表面稳定,不易掉落,所述的制得一定浓度的二茂铁-氧化石墨烯复合物悬浮液,一定浓度为2mg/ml。
5.如权利要求1所述一种比率电化学传感器用于检测对乙酰氨基苯酚的制备方法,其特征在于,步骤(5)中所述的取一定量(3)中制备悬浮液滴涂于预处理好的裸玻碳电极表面,一定量为3~5μL,所述磷酸盐缓冲溶液的pH为7.4且其浓度为5mM。
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