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Article(id=1240688791585878847, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1240688783964819588, articleNumber=null, orderNo=null, doi=10.16155/j.0254-1793.2024-0113, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1708617600000, receivedDateStr=2024-02-23, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773732858797, onlineDateStr=2026-03-17, pubDate=1727625600000, pubDateStr=2024-09-30, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773732858797, onlineIssueDateStr=2026-03-17, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773732858797, creator=13701087609, updateTime=1773732858797, updator=13701087609, issue=Issue{id=1240688783964819588, tenantId=1146029695717560320, journalId=1205117023404326918, year='2024', volume='44', issue='9', pageStart='1463', pageEnd='1645', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773732856979, creator=13701087609, updateTime=1773733032821, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1240689521587712627, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1240688783964819588, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1240689521587712628, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1240688783964819588, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=1638, endPage=1645, ext={EN=ArticleExt(id=1240688793108411219, articleId=1240688791585878847, tenantId=1146029695717560320, journalId=1205117023404326918, language=EN, title=Determination of vanillic acid based on POM-host guest materials, columnId=1240688788851183859, journalTitle=Chinese Journal of Pharmaceutical Analysis, columnName=Quality Control·Research Technolog, runingTitle=null, highlight=null, articleAbstract=

Objective: To determine the concentration of vanillic acid by polyoxometal-based host-guest frame material modified glass carbon electrode. Methods: A stable polyacid-based host-guest metal-organic framework material PMoV@MIL-100(Fe) was synthesized by combining vanadium-substituted phosphomolybdic acid (PMoV) with MIL-100(Fe) according to the synthesis method of polyacid-based host-guest framework materials. Functional composite material PMoV@MIL-100(Fe)@Pt was prepared by composite metal nanoparticles with PMoV@MIL-100(Fe) by solution method, and was used to modify glassy carbon electrode, detect vanillic acid, and prepare vanillic acid electrochemical sensor. Results: Under optimal conditions, the vanillic acid electrochemical sensor showed wide linear range and high sensitivity. Rapid and sensitive detection of vanillic acid could be performed under mild conditions with excellent stability. Conclusion: The electrochemical sensor constructed in this experiment provides a new idea for the detection of vanillic acid.

, correspAuthors=Cong ZHANG, Hai-yan ZHAO, Huan ZHANG, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, authorCompany=null, fund=null, authors=null, authorsList=Na LI, Shi-xu CHEN, Cong ZHANG, Hai-yan ZHAO, Min CUI, Bao SUN, Hua-fan LI, Huan ZHANG), CN=ArticleExt(id=1240688795423667197, articleId=1240688791585878847, tenantId=1146029695717560320, journalId=1205117023404326918, language=CN, title=基于多酸主客体材料在检测香草酸中的应用, columnId=1240688789006373124, journalTitle=药物分析杂志, columnName=质量评价·技术研发, runingTitle=null, highlight=null, articleAbstract=

目的：采用多金属氧酸盐基主客体框架材料修饰玻碳电极测定香草酸的浓度。方法：按照多酸基主客体框架材料合成方法，选择钒取代的磷钼酸(PMoV)与MIL-100(Fe)复合，合成了一种稳定的基于多酸的主客体金属有机框架材料PMoV@MIL-100(Fe)。通过溶液法将金属纳米粒子与PMoV@MIL-100(Fe)复合，制备功能性复合材料PMoV@MIL-100(Fe)@Pt，并用来修饰玻碳电极，检测香草酸，制备香草酸电化学传感器。结果：在最佳条件下，该香草酸电化学传感器表现出宽的线性范围和较高灵敏度。可以在温和的条件下对香草酸进行快速灵敏的检测，且具有出色的稳定性。结论：本实验构建的电化学传感器为检测香草酸提供了新思路。

, correspAuthors=张聪, 赵海燕, 张焕, authorNote=null, correspAuthorsNote=
** 张聪　Tel: (0311)81669959; E-mail: ;
赵海燕　Tel: （0311）81669959; E-mail: ;
张焕　Tel: （0311）69095009; E-mail:
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Tel: (0311)81669959; E-mail:

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Tel: (0311)81669959; E-mail:

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A.全谱(full spectrum)　B.C1s　C.O1s　D.Fe2p　E.Mo3d　F.V2p

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1~10.不同干扰物（different distractors）

, figureFileSmall=g7H9PljjBWP25Hk/MxZIeg==, figureFileBig=7GiQysQIahcVXylcOkN4IA==, tableContent=null), ArticleFig(id=1240704460293460638, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688791585878847, language=EN, label=Tab.1, caption=

The recovery test

, figureFileSmall=null, figureFileBig=null, tableContent=
样品
（sample）		加入值
（added）/(μmol·L-1)		测定值
(found)/(μmol·L-1)		回收率
(recovery)/%		RSD/%
湖水(lake water)50.052.79105.61.2
75.075.09100.11.6
100.095.6295.62.7
自来水(tap water)50.050.33100.72.3
75.076.59102.11.7
100.095.7395.71.6
), ArticleFig(id=1240704460381541026, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1240688791585878847, language=CN, label=表1, caption=

回收率检测

, figureFileSmall=null, figureFileBig=null, tableContent=
样品
（sample）		加入值
（added）/(μmol·L-1)		测定值
(found)/(μmol·L-1)		回收率
(recovery)/%		RSD/%
湖水(lake water)50.052.79105.61.2
75.075.09100.11.6
100.095.6295.62.7
自来水(tap water)50.050.33100.72.3
75.076.59102.11.7
100.095.7395.71.6
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基于多酸主客体材料在检测香草酸中的应用
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李娜 1 , 陈世旭 1 , 张聪 1, ** , 赵海燕 1, ** , 崔敏 1 , 孙宝 1 , 李化凡 1 , 张焕 2, **
药物分析杂志 | 质量评价·技术研发 2024,44(9): 1638-1645
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药物分析杂志 | 质量评价·技术研发 2024, 44(9): 1638-1645
基于多酸主客体材料在检测香草酸中的应用
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李娜1 , 陈世旭1, 张聪1, ** , 赵海燕1, ** , 崔敏1, 孙宝1, 李化凡1, 张焕2, **
作者信息
  • 1.河北科技大学理学院河北省表界面光电调控重点实验室，石家庄　050018
  • 2.河北省中医院，石家庄　050018

    • Tel: (0311)81669959; E-mail:

通讯作者:

** 张聪　Tel: (0311)81669959; E-mail: ;
赵海燕　Tel: （0311）81669959; E-mail: ;
张焕　Tel: （0311）69095009; E-mail:
Determination of vanillic acid based on POM-host guest materials
Na LI1 , Shi-xu CHEN1, Cong ZHANG1, ** , Hai-yan ZHAO1, ** , Min CUI1, Bao SUN1, Hua-fan LI1, Huan ZHANG2, **
Affiliations
  • 1.Hebei Provincial Key Laboratory of Photoelectric Control on Sunface and Interface, College of Science, Hebei University of Science and Technology, Shijiazhuang 050018, China
  • 2.Hebei Province Chinese Medicine Hospital, Shijiazhuang 050018, China
出版时间: 2024-09-30 doi: 10.16155/j.0254-1793.2024-0113
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摘要
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目的：采用多金属氧酸盐基主客体框架材料修饰玻碳电极测定香草酸的浓度。方法：按照多酸基主客体框架材料合成方法，选择钒取代的磷钼酸(PMoV)与MIL-100(Fe)复合，合成了一种稳定的基于多酸的主客体金属有机框架材料PMoV@MIL-100(Fe)。通过溶液法将金属纳米粒子与PMoV@MIL-100(Fe)复合，制备功能性复合材料PMoV@MIL-100(Fe)@Pt，并用来修饰玻碳电极，检测香草酸，制备香草酸电化学传感器。结果：在最佳条件下，该香草酸电化学传感器表现出宽的线性范围和较高灵敏度。可以在温和的条件下对香草酸进行快速灵敏的检测，且具有出色的稳定性。结论：本实验构建的电化学传感器为检测香草酸提供了新思路。

多金属氧酸盐  /  香草酸  /  电化学传感器  /  主客体  /  多金属氧酸盐的金属有机骨架结构

Objective: To determine the concentration of vanillic acid by polyoxometal-based host-guest frame material modified glass carbon electrode. Methods: A stable polyacid-based host-guest metal-organic framework material PMoV@MIL-100(Fe) was synthesized by combining vanadium-substituted phosphomolybdic acid (PMoV) with MIL-100(Fe) according to the synthesis method of polyacid-based host-guest framework materials. Functional composite material PMoV@MIL-100(Fe)@Pt was prepared by composite metal nanoparticles with PMoV@MIL-100(Fe) by solution method, and was used to modify glassy carbon electrode, detect vanillic acid, and prepare vanillic acid electrochemical sensor. Results: Under optimal conditions, the vanillic acid electrochemical sensor showed wide linear range and high sensitivity. Rapid and sensitive detection of vanillic acid could be performed under mild conditions with excellent stability. Conclusion: The electrochemical sensor constructed in this experiment provides a new idea for the detection of vanillic acid.

polyoxometallate  /  vanillic acid  /  electrochemical sensor  /  host-guest  /  POMOFs
李娜, 陈世旭, 张聪, 赵海燕, 崔敏, 孙宝, 李化凡, 张焕. 基于多酸主客体材料在检测香草酸中的应用. 药物分析杂志, 2024 , 44 (9) : 1638 -1645 . DOI: 10.16155/j.0254-1793.2024-0113
Na LI, Shi-xu CHEN, Cong ZHANG, Hai-yan ZHAO, Min CUI, Bao SUN, Hua-fan LI, Huan ZHANG. Determination of vanillic acid based on POM-host guest materials[J]. Chinese Journal of Pharmaceutical Analysis, 2024 , 44 (9) : 1638 -1645 . DOI: 10.16155/j.0254-1793.2024-0113
正文
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香草酸(vanillic acid，4-羟基-3-甲氧基苯甲酸)是一种含有酚酸结构的化合物，一般来源于水果、植物和蔬菜的次生代谢具有清除自由基和抗癌特性以及抗糖尿病、抗氧化、抗菌或抗炎作用[1-3]。香草酸被广泛用作食品的添加剂，主要用于增强食品的香气和口味。它可以用于调味剂的制备，如植物提取物、果脯等。此外，香草酸还可以用作食品的防腐剂，延长食品的保鲜期。并且，香草酸是胡黄连的抗菌成分之一，测定胡黄连所含的香草酸量，可以作为衡量胡黄连质量的指标[4]，因此需要开发合适的分析方法来有效地检测和定量复杂基质中的这种酚类化合物。目前检测香草酸的方法有高效液相色谱法[5-7]、毛细电泳法[8]、光谱法[9]和电化学检测方法[10-11]。其中电化学检测方法相较于其他测试手段，具有耗时少、操作简单、成本低、灵敏度高的优点[12-13]。此外，电化学检测方法可以通过不同材料对电极表面进行修饰，从而增强分析检测能力。
多金属氧酸盐(polyoxometalates，POMs)是一类过渡金属氧簇，不仅具有丰富的结构多功能性，而且具有优异的氧化还原特性，在催化、医学和生物学等研究领域有着广泛的应用[14-17]。更重要的是，通过调节溶液的pH或离子强度，可控地去除多金属氧酸盐中1个、2个或多个补位金属原子，引入其他金属原子形成取代的多金属氧酸盐[18]。钒是常见的杂原子，Keggin结构取代原子的氧化能力大小顺序为V、Mo、W[19]，因此，钒原子引入经典的多酸结构中形成钒取代的多阴离子，可以提高多阴离子的表面电荷密度[20-22]，提高多金属氧酸盐的氧化还原活性，并且丰富多酸的电化学性能[23]。然而多金属氧酸盐在电解液中部分溶解，限制了其应用。克服这些缺点的策略之一是将它们封装在多孔框架结构中。
最近，许多研究学者报道了基于多金属氧酸盐的金属有机骨架结构(POMOFs)的研究[24]，多金属氧酸盐作为客体分子封装在孔中。例如，MIL-100(Fe)是一种立方三维多孔Fe3+基金属有机骨架，以铁(Ⅲ)八面体为氧中心三聚体，以三聚体阴离子(1，3，5-苯三甲酸)通过配位键构建而成[24-25]。MIL-100(Fe)允许在其更大的介孔笼中轻松地封装多金属氧酸盐。这种核/壳结构的多金属氧酸盐基MOF复合材料不仅具有较大的表面积，为电子和离子提供了方便的传输途径，而且其多组分和多界面的结构在电化学过程中诱导了电子的协同传递和潜在的质量传递，这有助于提高整个电极的电化学性能和稳定性。
同时加入金属纳米粒子以提高整体的导电性[26-27]，金属纳米粒子材料具有优异的催化性能及良好的导电性和稳定性。这些优异的性能使得金属纳米粒子在电化学传感领域广泛应用[28]。
因此，本实验制备了基于钒取代磷钼酸(PMoV)的MIL-100(Fe)与Pt纳米粒子复合材料，以此修饰电极构建了电化学传感器，该传感器可以有效地检测香草酸，同时该传感器具有灵敏度高、线性范围宽、回收率好、重现性高等特点。
1　仪器与试药
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JEM-2100型透射电镜 (TEM)（JEOL公司），S-4800型扫描电镜 (SEM)（HITACHI公司），D/max-rA 型X-射线粉末衍射 (XRD)（Rigaku公司），TENSOR 37型傅立叶变换红外光谱仪 (FT-IR)（Bruker公司）和250Xi型X-射线光电子能谱仪 (XPS)（Escalab公司）。分析纯偏钒酸钠(NaVO3)、钼酸钠(Na2MoO4·H2O)、十二水磷酸钠(Na3PO4·12H2O)和硼氢化钠(NaBH4)购自上海阿拉丁化学有限公司。分析纯六氯铂酸钾(K2PtCl6)购自Sigma-Aldrich公司。分析纯磷酸氢二钠（Na2HPO4）和磷酸二氢钠（NaH2PO4）购自天津达茂化学试剂有限公司。所有试剂没有进一步处理。所有水溶液均用二次水配制。所有的电化学实验是在电化学工作站 (CHI660D，上海)上进行的。使用三电极体系：修饰电极为工作电极，铂丝电极为对电极 (1 mm)，Ag/AgCl电极(饱和KCl) 为参比电极。
2　方法
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2.1　PMoV的制备[21]
称取1.22 g NaVO3溶于20 mL去离子水中，将Na3PO4·12H2O 3.8 g溶于50 mL 去离子水并缓慢滴加到上述溶液中。用1∶1稀H2SO4调节pH至5，在90 ℃下加热混合溶液30 min。加Na2MoO4·2H2O 24.2 g于上述反应液中，调pH至2.5，继续加热180 min，冷却至室温。在含有稀H2SO4的乙醚中萃取、洗涤、干燥。
2.2　PMoV@MIL-100(Fe)的制备
根据文献[26]报道的方法，制备PMoV@MIL-100(Fe)。称取FeCl3·6H2O 1.62 g、均苯三甲酸0.68 g和PMoV 2.036 g溶于25 mL去离子水中，将上述溶液转移至聚四氟乙烯釜中。于130 ℃加热72 h后，将反应混合物冷却至室温，过滤并收集釜内沉淀。
2.3　PMoV@MIL-100(Fe)@Pt的制备
称取K2H6PtCl6 20 mg溶于10 mL去离子水中，搅拌1 h，逐滴加入新鲜制备的NaBH4水溶液，搅拌2 h，10 000 r·min-1离心10 min、水洗，在60 ℃下干燥[27]。配制1 mg·mL-1浓度的Pt纳米粒子分散液及PMoV@MIL-100(Fe)分散液，通过超声（60 W，40 kHz）混合，将一定比例的分散液混合均匀，制得PMoV@MIL-100(Fe)@Pt。
2.4　修饰电极的构建
本实验选用玻碳电极(GCE)。首先用氧化铝抛光粉在0.3和0.05 μm的绒布上进行连续打磨抛光。分别制备2 mg·mL-1的PMoV@MIL-100(Fe)、PMoV@MIL-100(Fe)@Pt水溶液并进行超声处理，直至形成均相溶液。取6 μL所制备的溶液滴涂到GCE电极表面，室温下自然晾干。分别记作PMoV@MIL-100(Fe)/GCE和PMoV@MIL-100(Fe)@Pt/GCE，将制作好的电极放在4 ℃下保存，备用。
3　结果与讨论
收起
3.1　TEM分析
为了观察合成材料的形貌，本实验采用TEM对形貌进行观察。从图1可以看到成功合成了PMoV@MIL-100(Fe)，其形貌为正四面体结构，与相关文献报道的一致，在加入Pt纳米粒子后可以观察到其均匀地分布在PMoV@MIL-100(Fe)四面体结构上。因此PMoV@MIL-100(Fe)@Pt复合材料制备成功。
3.2　红外分析
利用傅里叶变换红外光谱法对制备的PMoV和PMoV@MIL-100(Fe)进行了表征。以确定主要化学基团的存在，进而判断复合材料的合成情况。实验结果如图2所示，在1 060、961、865和762 cm-1处观测到4个吸收振动峰是由于P-Oc，Mo=Ot，Mo-Ob-Mo和Mo-Oe-Mo产生，这4个吸收振动峰是Keggin型PMoV的特征峰，其结果表明PMoV成功合成[23]。在PMoV@MIL-100(Fe)的谱图中，保留了PMoV4个特征峰的同时，在1708和1366 cm-1出现2个新的吸收峰是归因于来自芳香基团的n(C=O)和n(C-O)的拉伸振动。由此可以表明PMoV@MIL-100(Fe)已成功合成。
3.3　粉末X射线衍射分析
使用粉末X射线衍射(PXRD)对PMoV@MIL-100(Fe)和PMoV@MIL-100(Fe)@Pt进行表征(图3)。可以观察到样品PMoV@MIL-100(Fe)的特征峰与文献中报道的峰的位置一致[22]，表明PMoV@MIL-100(Fe)已成功合成。PMoV@MIL-100(Fe)和Pt纳米粒子复合后的XRD图谱表明在40°及48°位置出现新峰，根据相关文献，这2个峰归属于Pt纳米粒子的特征峰[28-29]。结果表明，PMoV@MIL-100(Fe)与Pt纳米粒子成功复合，同时Pt纳米粒子的加入并没有破坏PMoV@MIL-100(Fe)的结构。
3.4　X射线光电子能谱分析
为了进一步研究复合材料PMoV@MIL-100(Fe)，对复合材料进行了X射线光电子能谱(XPS)测试。如图4-A所示，在XPS中含有Fe、V、O、C、Mo和P元素[30]。如图4-B所示，C1s谱图中的峰出现在283.3 eV和287.2 eV处，分别对应于PMoV@MIL-100(Fe)中的C-C/C=C和O-C=O。图4(C)为O1s谱图，529.1 eV、530.5 eV和532.1 eV属于COOH、C=O和C-O。图4-D为Fe2p谱图，Fe2p1/2(724.1eV)和Fe2p3/2(710.4eV)2个峰，表明存在Fe3+。图4-E为Mo3d谱图，Mo3d的特征结合能为231.4 eV和234.5 eV的2个信号，分别对应于PMoV的Mo3d3/2和Mo3d5/2自旋轨道，表明样品中存在PMoV。图4(F)为V2p谱图，V2p的结合能在517eV的单个信号，可以证明PMoV中V原子成功取代。最终包含样品中的所有元素：来自MIL-100(Fe)的C、O和Fe元素，来自PMoV的P、Mo、V和O元素，这证实了PMoV@MIL-100(Fe)已成功制备。
3.5　修饰电极的电化学表征
利用电化学阻抗谱(EIS)进一步观察不同电极的导电性(图5)。实验在含5.0 mmol·L-1 [Fe(CN)6]3-/4-的0.1 mol·L-1氯化钾的溶液中进行，分别对GCE、PMoV@MIL-100(Fe)/GCE和PMoV@MIL-100(Fe)@Pt/GCE进行电化学表征。使用ZSimpWin软件等效电路模型模拟EIS数据，图中每条曲线半圆弧的直径的数值即为电极界面的极化电阻。在频率较高的情况下，由于极化影响较小，极化电阻即为电荷传递电阻(Rct)。经过模拟得出，GCE的Rct为130.6 Ω，用PMoV@MIL-100(Fe)修饰GCE后，修饰电极的Rct为160.6 Ω，这主要是因为PMoV@MIL-100(Fe)材料导电性差的原因，阻碍了电子的传递效率。当引入了PtNPs之后，PMoV@MIL-100(Fe)@Pt/GCE的Rct降低至78.9 Ω。综上所述，基于PtNPs和PMoV@MIL-100(Fe)所构建的复合材料具有优异的导电性，可以用于构建高效灵敏传感器。
3.6　可行性分析
利用CV法研究了不同修饰电极对香草酸的电化学行为。在含有浓度为200 μmol·L-1香草酸的B-R缓冲溶液(pH 2.5)中以不同修饰电极为工作电极进行CV测试，结果如图6-A所示，PMoV@MIL-100(Fe)@Pt/GCE有较高的峰电流信号，表明在复合材料修饰电极后对香草酸有较好的检测效果。为了进一步研究复合材料PMoV@MIL-100(Fe)@Pt的性能，判断PMoV@MIL-100(Fe)@Pt/GCE是否可以用于香草酸的定量检测，通过在不同浓度香草酸溶液中的电化学行为来判断。选择PMoV@MIL-100(Fe)@Pt/GCE为工作电极，利用DPV电化学方法分别在浓度为10、30、50和70 μmol·L-1香草酸的pH为2.5的B-R缓冲溶液中进行，实验结果如图6-B所示。随着溶液中香草酸浓度的增加，氧化峰电流也逐渐随之增加。这一现象表明，利用复合材料PMoV@MIL-100(Fe)@Pt作为电化学传感器的电极材料去定量检测香草酸的方案是可行的。
3.7　实验条件的优化
在不同的实验条件下，PMoV@MIL-100(Fe)@Pt/GCE修饰电极对香草酸的检测有不同的响应。因此，经实验探究，确定最佳实验条件：复合材料之间的比例为5.1，修饰电极的滴涂量为6 μL以及缓冲体系的pH为2.5。
3.8　香草酸的定量检测
本实验在最优条件下，用PMoV@MIL-100(Fe)@Pt修饰电极采用DPV法进行香草酸的定量检测，结果如图7-A所示。由图可知，香草酸在修饰电极上有良好的电化学响应，其氧化峰电流随浓度的增加而增加，在10~180和180~480 μmol·L-1呈现出两段良好的线性关系（图7-B）。其线性方程：
计算得出的检测限(S/N=3)为0.431 μmol·L-1。
3.9　修饰电极的选择性检测
为了检验修饰电极对香草酸的选择性，本实验采用DPV法，加入与香草酸的结构相似或可能对检测香草酸产生干扰的物质（如：对苯二酚、邻苯二酚、2，5-二羟基对苯二甲酸、对苯二甲酸、半胱氨酸、柠檬酸以及KCl、MgCl、CuNO3等），随着不同干扰物的加入，香草酸的峰电流几乎没有变化，并且在香草酸的出峰位置没有其他新峰出现，表明修饰电极对香草酸的检测没有干扰[31]。如图8所示。
3.10　修饰电极的重现性、重复性和稳定性
使用同一根电极经PMoV@MIL-100(Fe)@Pt多次修饰，以此电极检测同等浓度的香草酸，经过5次修饰后对香草酸的电化学响应基本一致，RSD为2.4%，说明重复性良好。在相同条件下，使用PMoV@MIL-100(Fe)@Pt修饰5根不同电极，RSD为2.2%，说明有较好的重现性。此外，每天测试同一根电极，连续测试10 d，电流响应仍能保持在88%以上。结果表明PMoV@MIL-100(Fe)@Pt修饰电极有良好的重复性和重现性，以及可接受的稳定性。
3.11　实际样品的检测
为了评估实际样品检测的可行性，使用PMoV@MIL-100(Fe)@Pt/GCE通过标准加入法检测湖水以及自来水中的香草酸。将不同已知浓度的香草酸加入到稀释后的溶液中，通过修饰电极检测样品中香草酸的浓度。结果表明，在湖水中的回收率在95.6%~105.6%，RSD在1.2%~2.6%；在自来水中的回收率在95.7%~102.1%，RSD在1.6%~2.3% (表1)。
4　结论
收起
本实验成功制备了PMoV@MIL-100(Fe)@Pt复合材料，并将其作为修饰材料修饰电极，成功构建了用于检测香草酸的电化学传感器。本实验选择钒取代的多金属氧酸盐通过主客体复合材料合成方案，将多酸封装进MIL-100(Fe)中，有效地解决了多金属氧酸盐在电解液中溶解度高的问题，同时随着Pt纳米粒子的加入，传感器的导电性增加。并且构建的电化学传感器具有较低的检出限和较高的灵敏度。此外，该传感器具有良好的重复性稳定性和抗干扰能力，可以用于香草酸的检测。本实验构建的电化学传感器为检测香草酸提供了新思路。
基金
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  • 河北省教育厅(BJK2023068)
  • 河北省省级科技计划项目(226Z7715G)
  • 河北省中医药管理局科研计划项目(2023039)
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2024年第44卷第9期
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doi: 10.16155/j.0254-1793.2024-0113
  • 接收时间：2024-02-23
  • 首发时间：2026-03-17
  • 出版时间：2024-09-30
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  • 收稿日期：2024-02-23
基金
河北省教育厅(BJK2023068)
河北省省级科技计划项目(226Z7715G)
河北省中医药管理局科研计划项目(2023039)
作者信息
    1.河北科技大学理学院河北省表界面光电调控重点实验室，石家庄　050018
    2.河北省中医院，石家庄　050018

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