Chinese Journal of Analytical Chemistry最新文献_第10页

Quality control methods established in view of the characteristics of component type of Yuhuang Shengji ointment based on HPLC, ICP-MS and GC e-nose 针对鱼黄生补软膏成分类型的特点，建立了HPLC、ICP-MS和GC电子鼻法的质量控制方法

IF 1.2 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-04-16 DOI: 10.1016/j.cjac.2025.100550

Kewei WANG , Ying ZHANG , Xilong QIAN , Zheng LIU , Weihua ZHANG , Liu ZHOU , Yanqiong PAN , Liwen ZHENG , Fang FANG , Yang ZHANG , Yehuang WANG , Bin JIANG , Shengjin LIU

Yuhuang Shengji ointment (YSO) is a traditional Chinese medicine clinical prescription from Professor Wang Yehuang, a famous Chinese medicine professor in Jiangsu Province, China. It is used for the treatment of postoperative healing of anal fistula in clinic practice. It is composed of Corydalis Rhizoma, Radix Sanguisorbae Carbonisata, Natrii Sulfas, Alumen Ustum, Plant Soot and Borneolum. It has the effects of eliminating dampness, astringing sores, hemostasis, pain relief, detumescence and muscle regeneration. According to the characteristics that YSO mainly contains inorganic, organic and volatile components, the comprehensive quality control of the ointment was achieved by different analytical methods. The organic components in the ointment were qualitatively analyzed by ultra performance liquid chromatography coupled with quadrupole time of flight mass spectrometry (UPLC-Q-TOF-MS) to determine the main chemical components. High performance liquid chromatography (HPLC) fingerprint of the organic components of the ointment was further established. Inductively coupled plasma mass spectrometry (ICP-MS) technology is used to analyze the inorganic elements in ointment, which provides data support for the quality control of inorganic components. The flash GC e-nose is used for rapid detection of volatile substances in ointment, and the fingerprint of volatile components is established. The comprehensive use of these analytical techniques not only reflects the overall chemical characteristics of the ointment, but also helps to evaluate the consistency between different batches of products. This study successfully established a comprehensive quality analysis method, which provided a basis for the quality control of YSO. At the same time, it provides a more comprehensive quality control strategy for ointment which mainly contains organic, inorganic and volatile components.

御黄生机软膏（YSO）是中国江苏省著名中医教授王业黄教授的一款中药临床处方。临床上多用于肛瘘术后愈合的治疗。主要成分为延胡索、三地血根、苦钠、铝叶、植物烟灰、冰片。具有祛湿、收敛疮、止血、止痛、消肿、肌肉再生等功效。根据YSO主要含有无机、有机和挥发性成分的特点，采用不同的分析方法实现了软膏的综合质量控制。采用超高效液相色谱联用四极杆飞行时间质谱（UPLC-Q-TOF-MS）对软膏中的有机成分进行定性分析，确定其主要化学成分。进一步建立了软膏中有机成分的高效液相色谱指纹图谱。采用电感耦合等离子体质谱（ICP-MS）技术对软膏中的无机元素进行分析，为软膏中无机成分的质量控制提供数据支持。采用闪蒸气相色谱电子鼻对药膏中挥发性物质进行快速检测，建立了挥发性成分指纹图谱。综合运用这些分析技术，不仅能反映软膏的整体化学特性，而且有助于评价不同批次产品之间的一致性。本研究成功地建立了一种综合质量分析方法，为青苏子的质量控制提供了依据。同时为以有机、无机和挥发性成分为主的软膏提供了更全面的质量控制策略。

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引用次数: 0

Synthesis of carbon dots based on chitosan and melamine and their application in detecting vanadate (V) anions 壳聚糖和三聚氰胺碳点的合成及其在钒酸盐阴离子检测中的应用

IF 1.2 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-04-14 DOI: 10.1016/j.cjac.2025.100538

Farida ALLAMBERGENOVA , Zulayho SMANOVA , Nigora QUTLIMUROTOVA , Abdurakhman ABDREYMOV , Fotima SOBIROVA , Ruhiya QUTLIMUROTOVA , Khusan YAKHSHINOROV

Vanadium is considered a microelement of great industrial, environmental, biological, and pharmacological importance. Vanadium-containing complexes have been widely used as biologically active compounds. Outside cells, vanadium exists in the form of the vanadate anion, while inside cells, it primarily exists as the tetravalent vanadyl cation. Both a deficiency and an excess of vanadium in the human body can lead to various diseases. Therefore, the aim of this study is to detect vanadium (V) ions using fluorescent carbon dots, which are capable of rapid and sensitive detection. In this study, carbon dots synthesized from chitosan and melamine were used as fluorescent reagents. Fluorescent carbon dots (C-dots) were synthesized by hydrothermally treating 99.95% pure chitosan with melamine at 180 °C for 5 h, followed by freeze-drying in a lyophilizer, and purification using high performance liquid chromatography (HPLC). These dots were found to emit bright green fluorescence. The formation of green fluorescence is associated with the incorporation of nitrogen into the carbon materials, which were then used for the detection of vanadium (V) ions. The C-dots and their complexation with vanadium (V) were fully characterized by infrared spectroscopy and spectrofluorometry.

钒被认为是一种具有重要工业、环境、生物和药理意义的微量元素。含钒配合物作为生物活性化合物得到了广泛的应用。在细胞外，钒以钒酸盐阴离子的形式存在，而在细胞内，钒主要以四价钒基阳离子的形式存在。人体内的钒缺乏和过量都会导致各种疾病。因此，本研究的目的是利用荧光碳点检测钒(V)离子，该方法具有快速、灵敏的检测能力。本研究以壳聚糖和三聚氰胺合成碳点作为荧光试剂。用三聚氰胺对99.95%纯度的壳聚糖进行180℃水热处理5 h，冷冻干燥，高效液相色谱（HPLC）纯化，合成荧光碳点（C-dots）。这些点被发现发出明亮的绿色荧光。绿色荧光的形成与碳材料中氮的掺入有关，然后用于检测钒(V)离子。用红外光谱和荧光光谱法对c点及其与钒(V)的络合进行了表征。

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引用次数: 0

A novel coumarin-thiazole conjugated ICT fluorescent probe for cysteine specific detection in food samples, living cells and zebrafish 一种新型香豆素-噻唑偶联ICT荧光探针，用于食品样品、活细胞和斑马鱼中半胱氨酸的特异性检测

IF 1.2 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-04-14 DOI: 10.1016/j.cjac.2025.100542

Xiaoyan CAO, Yifan WEI, Yingyue DING, Yichi ZHANG, Chuanqing REN, Qin WANG

Inspired by the advantageous properties of coumarin and thiazole fluorophores, we rationally designed and developed a novel coumarin-thiazole conjugated fluorescent probe (PC), featuring an acryloyl ester group as the triggering and responding entity for the specific identification of cysteine (Cys). Probe PC exhibited a distinct color change (colorless to bright green), a large Stokes shift, excellent sensitivity, high selectivity, and strong anti-interference capabilities. the density function theory (DFT), high-resolution mass spectrometry (HRMS), and proton nuclear magnetic resonance (¹H NMR) assays further affirmed that the response mechanism encompasses an addition-cyclization reaction between the acryloyl domain of probe PC and the sulfhydryl and amino entities of Cys, engendering the liberation of a lustrous green fluorescent chromophore (PCOH) that can be visually discerned. Compared with previous reports, this is a new scaffold based on coumarin that achieves the quantitative determination of Cys in different food matrices in real-time. Furthermore, probe PC is effectively employed for visual imaging of Cys in A549 cells and five-day-old zebrafish, exhibiting low cytotoxicity and favorable cellular permeability, which demonstrated its practical application.

受香豆素和噻唑荧光团的优势特性启发，我们合理设计并开发了一种新型的香豆素-噻唑共轭荧光探针（PC），该探针以丙烯酰酯基为触发和响应实体，对半胱氨酸（Cys）进行特异性鉴定。探针PC表现出明显的颜色变化（无色到亮绿色），Stokes位移大，灵敏度好，选择性高，抗干扰能力强。密度泛函理论（DFT）、高分辨率质谱分析（HRMS）和质子核磁共振（1H NMR）进一步证实了响应机制包括探针PC的丙烯基结构域与Cys的巯基和氨基实体之间的加成-环化反应，从而释放出具有光泽的绿色荧光发色团（PCOH）。与以往报道相比，这是一种基于香豆素的新型支架，实现了不同食物基质中Cys的实时定量测定。此外，探针PC有效地用于A549细胞和5日龄斑马鱼的Cys视觉成像，具有低细胞毒性和良好的细胞通透性，证明了其实际应用价值。

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引用次数: 0

Determination of illicit drugs in sediments using a modified QuEChERS method coupled with UPLC-MS/MS 改良QuEChERS - UPLC-MS/MS法测定沉积物中违禁药物

IF 1.2 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-04-14 DOI: 10.1016/j.cjac.2025.100540

Meng ZHANG, Changsheng GUO, Heng ZHANG, Yanghui DENG, Xu TAN, Ya GAO, Jian XU

The occurrence of illicit drugs in water has been extensively reported around the world, however, limited data are available in sediments, probably due to the lack of effective and robust analytical methods. This research established a sensitive method for determining 12 illicit drugs, including amphetamine, methamphetamine, methcathinone, ephedrine, 3,4-methylenedioxy-amphetamine, 3,4-methylenedioxy-n-methamphetamine, norketamine, ketamine, benzoylecgonine, codeine, cocaine, and methadone in sediments. The combination of salt and solution (extraction step) and adsorbents (purification step) in the QuEChERS method was optimized to enhance the applicability and reliability of the analytical approach, which was subsequently combined with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The developed method demonstrated satisfactory linearity (R² > 0.995) within 0.1 to 50 ng/g dry weight (dw), with limits of detection and quantification ranging from 0.0077 to 0.0299 ng/g dw and 0.0255 to 0.0996 ng/g dw, respectively. Recoveries of target drugs ranged from 60.5 % to 114.9 %, with intra-day and inter-day relative standard deviations below 10.9 % and 12.3 %, respectively, which are within the acceptable limits. Application of the validated method to sediments from the Beiyunhe River Basin, China revealed the presence of nine out of twelve targeted drugs. Total drug concentrations ranged from 0.12 to 1.18 ng/g dw, with ephedrine being predominant, followed by amphetamine and methadone. Ecological risk assessments indicated low biological hazards from the detected drugs to aquatic ecosystems. However, due to their high polarity and biological activity, continued attention to the ecological risks of illicit drugs would provide greater reassurance. This research presents the first application of QuEChERS for extracting illicit drugs from sediments. The optimized method elucidates these emerging contaminants' behavior and facilitates accurate environmental risk assessments. Due to its high sensitivity, good recovery and precision, the method is well-suited to routine monitoring of trace-level illicit drugs in complex sediment matrices.

世界各地广泛报道了水中存在非法药物的情况，但沉积物的数据有限，这可能是由于缺乏有效和可靠的分析方法。本研究建立了测定沉积物中安非他命、甲基苯丙胺、甲卡西酮、麻黄碱、3,4-亚甲基二氧基苯丙胺、3,4-亚甲基二氧基-n-甲基苯丙胺、去氯胺酮、氯胺酮、苯甲酰ecgonine、可待因、可卡因、美沙酮等12种违禁药物的灵敏方法。优化了QuEChERS方法中盐溶液（萃取步骤）和吸附剂（纯化步骤）的组合，提高了分析方法的适用性和可靠性，并将其与超高效液相色谱-串联质谱（UPLC-MS/MS）相结合。所开发的方法具有良好的线性(R2 >；0.995)在0.1 ~ 50 ng/g干重（dw）范围内，检测限和定量限分别为0.0077 ~ 0.0299 ng/g dw和0.0255 ~ 0.0996 ng/g dw。加样回收率为60.5% ~ 114.9%，日内、日内相对标准偏差分别小于10.9%和12.3%，均在可接受范围内。将该方法应用于中国北云河流域的沉积物中，发现12种靶向药物中有9种存在。药物总浓度范围为0.12 ~ 1.18 ng/g dw，以麻黄碱为主，其次为安非他明和美沙酮。生态风险评价表明，检测到的药物对水生生态系统的生物危害较低。然而，由于非法药物的高极性和生物活性，继续注意其生态风险将提供更大的保证。本研究首次应用QuEChERS从沉积物中提取违禁药物。优化后的方法阐明了这些新出现的污染物的行为，有助于准确的环境风险评估。该方法灵敏度高，回收率好，精密度高，适用于复杂沉积物基质中痕量违禁药物的常规监测。

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引用次数: 0

Steric and energetic studies on the retention of Cd (II) and Zn (II) metal ions into magnesium rich zeolite-A synthesized from natural talc: Experimental and theoretical studies

IF 1.2 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-04-13 DOI: 10.1016/j.cjac.2025.100541

Walaa GABER , Nabila SHEHATA , May BIN-JUMAH , Ahmed A. ALLAM , Wail Al ZOUBI , Mostafa R. ABUKHADRA

Magnesium-rich zeolite-A (Mg.ZA) was successfully synthesized from natural talc minerals as a novel form of magnesium silicate zeolitic structure with a surface area of 187 m²/g and mesoporous nature (1.5 to 10 nm). Different characterization techniques, including X-ray diffraction (XRD), fourier transform infrared spectroscopy (FT-IR), energy dispersive X-ray spectroscopy (EDX), scanning electron microscope (SEM), and Brunner−Emmet−Teller (BET), confirmed the formation of Mg.ZA. The adsorption properties of Mg.ZA were evaluated for effective retention of toxic Cd (II) and Zn (II) metallic ions from the water supplies. The Mg.ZA structure displays significant capacities for the two ions, with saturation capacities (278 mg/g (Cd (II)) and 221.2 mg/g (Zn (II)) higher than several investigated adsorbents. Based on the steric analysis of the applied advanced isotherm models, the structure of Mg.ZA was enriched in 150 and 106.9 mg/g effective uptake sites during the retention of Cd (II) and Zn (II), respectively. Up to three ions of Cd (II) and Zn (II) can occupy each of these sites, contributing to their adsorption in a vertical orientation through multi-interaction or multi-ionic mechanisms. The energetic assessment, either based on Gaussian energy (< 7 kJ/mol) or adsorption energy (< 6 kJ/mol), suggested the predominant impact of physical mechanisms (hydrogen bonds and electrostatic attraction), in addition to the impact of the zeolitic ion exchange process (0.6 to 25 kJ/mol). Furthermore, the thermodynamic functions declare the retention of these ions into the framework of Mg.ZA by exothermic and spontaneous reactions.

富镁沸石a （Mg.ZA）是一种新型的镁硅酸盐沸石结构，具有介孔性质（1.5 ~ 10 nm），比表面积为187 m2/g。不同的表征技术，包括x射线衍射（XRD）、傅里叶变换红外光谱（FT-IR）、能量色散x射线光谱（EDX）、扫描电子显微镜（SEM）和Brunner - Emmet - Teller (BET)，证实了Mg.ZA的形成。镁的吸附性能。评估了ZA对水中有毒Cd （II）和Zn （II）金属离子的有效保留。Mg。ZA结构对两种离子表现出显著的吸附能力，其饱和容量(278 mg/g （Cd (II)）和221.2 mg/g （Zn (II)）高于几种所研究的吸附剂。基于已应用的先进等温线模型的立体分析，研究了镁合金的结构。在Cd （II）和Zn （II）滞留过程中，ZA分别富集于150和106.9 mg/g有效摄取位点。Cd （II）和Zn （II）离子最多可以占据三个位点，通过多相互作用或多离子机制在垂直方向上吸附它们。能量评估，要么基于高斯能量(<；7kj /mol)或吸附能(<；6 kJ/mol)，表明除了沸石离子交换过程（0.6 ~ 25 kJ/mol）的影响外，物理机制（氢键和静电吸引）也是主要的影响因素。此外，热力学函数表明这些离子保留在Mg的框架内。放热反应和自发反应。

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引用次数: 0

Development and validation of an HPLC method for quantitative analysis of trigonelline 葫芦巴碱HPLC定量分析方法的建立与验证

IF 1.2 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-04-10 DOI: 10.1016/j.cjac.2025.100530

Ming BAI, Xuebing LI, Yawen LIU, Liwei ZHAO, Qingqi FENG, Jianlong MA

Trigonelline is an alkaloid primarily found in fenugreek (Trigonella foenum-graecum) seeds, exhibiting diverse pharmacological activities, including anti-diabetic, antioxidant, and anti-inflammatory effects. With the growing application of trigonelline in drug development and quality control, the development of efficient and accurate analytical methods is critical to ensure its proper assessment and utilization. This study aims to develop and validate a HPLC method for the precise separation and quantitative determination of trigonelline. The method utilizes a Dalian Elite Hypersil NH₂ chromatographic column (250 mm × 4.6 mm, 5 µm) with a mobile phase of acetonitrile: water (70:30, v/v), a flow rate of 1.0 mL/min, column temperature maintained at 35 °C, and detection wavelength set at 264 nm. The method was applied to analyze fenugreek seed extracts prepared via ultrasonic extraction with methanol, employing a 30-minute extraction time. The results demonstrated that the method achieved an excellent linear range (R² > 0.9999), high precision (RSD < 2 %), system suitability, and recovery rate is between 95 % and 105 %, meeting the quality standards for trigonelline analysis. In conclusion, this study introduces a reliable and efficient HPLC method, offering robust technical support for the quantitative analysis of trigonelline and the quality evaluation of related pharmaceutical products, facilitating its application in clinical drug monitoring and standardization.

葫芦巴碱是一种主要存在于葫芦巴种子中的生物碱，具有多种药理活性，包括抗糖尿病、抗氧化和抗炎作用。随着葫芦巴碱在药物开发和质量控制中的应用越来越广泛，建立高效、准确的分析方法是保证其合理评价和利用的关键。本研究旨在建立高效液相色谱法精确分离和定量测定葫芦巴碱。方法采用大连Elite Hypersil NH2色谱柱（250 mm × 4.6 mm, 5µm），流动相为乙腈：水（70:30,v/v），流速为1.0 mL/min，柱温35℃，检测波长264 nm。采用该方法对甲醇超声提取胡芦巴籽提取物进行了分析，提取时间为30分钟。结果表明，该方法具有良好的线性范围(R2 >；0.9999)，高精度(RSD <；回收率在95 % ~ 105 %之间，符合葫芦巴碱分析的质量标准。综上所述，本研究引入了一种可靠、高效的HPLC方法，为葫芦巴碱的定量分析和相关药品的质量评价提供了有力的技术支持，促进了葫芦巴碱在临床药物监测和标准化中的应用。

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引用次数: 0

Network pharmacology-based identification of key pharmacological pathways of epimedium acting on hepatocellular carcinoma 基于网络药理学的淫羊藿作用于肝癌的关键药理通路鉴定

IF 1.2 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-04-07 DOI: 10.1016/j.cjac.2025.100532

Mei YAN , Guanping LAI , Renzhong XIAO

Epimedium (Epimedium Tourn. ex L.), a traditional Chinese herb, is known for its kidney-nourishing and Yang-reinforcing properties. Its flavonoids exhibit potential anticancer properties. Nevertheless, the precise mechanisms through which epimedium impacts hepatocellular carcinoma (HCC) remain unclear. To elucidate these mechanisms, we employed a network pharmacology strategy. Active ingredients of epimedium were identified from the Traditional Chinese Medicine Systems Pharmacology Database and Analysis Platform database, whereas HCC-associated genes were extracted from five different databases. Protein-protein interaction networks were constructed using the STRING database, followed by Gene Ontology and Kyoto Encyclopedia of Genes and Genomes pathway analyses using the Database for Annotation, Visualization, and Integrated Discovery platform. Network analyses were conducted using Cytoscape 3.8.0 and R 4.0.4 with the Bioconductor package. Our findings revealed 23 active ingredients and 65 common targets in HCC, potentially modulating core targets, such as Cellular tumor antigen p53, Vascular endothelial growth factor A, RAC-alpha serine/threonine-protein kinase, Insulin-like growth factor 1 receptor, and Hepatocyte growth factor receptor. Chryseriol, luteolin, and kaempferol emerged as the top three core components affecting cancer pathways. Molecular docking studies confirmed that these ingredients effectively bind to the aforementioned targets. In summary, the therapeutic benefits of epimedium in HCC are likely attributed to bioactive ingredients such as chryseriol, luteolin, and kaempferol, which facilitate apoptosis in HCC cells. These ingredients also modulate crucial cancer-related pathways, including pidermal growth factor receptor tyrosine kinase inhibitor resistance, PI3K-Akt signaling, and vascular endothelial growth factor signaling. This study offers valuable insights into the pharmacological mechanisms underlying epimedium’s effects in HCC, highlighting its potential as a promising therapeutic agent.

淫羊藿（淫羊藿）（如L.），一种传统的中国草药，以其滋肾补阳的特性而闻名。它的类黄酮具有潜在的抗癌特性。然而，epimedium影响肝细胞癌（HCC）的确切机制尚不清楚。为了阐明这些机制，我们采用了网络药理学策略。从中药系统药理学数据库和分析平台数据库中鉴定淫羊藿的有效成分，从5个不同的数据库中提取hcc相关基因。利用STRING数据库构建蛋白-蛋白互作网络，利用database for Annotation、Visualization和Integrated Discovery平台对基因本体和京都基因与基因组百科全书进行路径分析。使用Cytoscape 3.8.0和r4.0.4以及Bioconductor软件包进行网络分析。我们的研究结果揭示了23种有效成分和65种HCC常见靶点，潜在调节核心靶点，如细胞肿瘤抗原p53、血管内皮生长因子A、rac - α丝氨酸/苏氨酸蛋白激酶、胰岛素样生长因子1受体和肝细胞生长因子受体。金缕木酚、木犀草素和山奈酚是影响癌症途径的三大核心成分。分子对接研究证实，这些成分与上述靶点有效结合。综上所述，淫羊藿在HCC中的治疗作用可能归因于其生物活性成分，如金苍酚、木犀草素和山奈酚，它们促进了HCC细胞的凋亡。这些成分还可以调节关键的癌症相关通路，包括表皮生长因子受体酪氨酸激酶抑制剂耐药性、PI3K-Akt信号和血管内皮生长因子信号。本研究为淫羊藿在HCC中作用的药理学机制提供了有价值的见解，突出了其作为一种有前景的治疗剂的潜力。

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引用次数: 0

Analytical strategies for quantifying methylated selenium species in staple crops: Methods, and emerging techniques 主食作物中甲基化硒的定量分析策略：方法和新兴技术

IF 1.2 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-04-01 DOI: 10.1016/j.cjac.2025.100511

Angstone Thembachako MLANGENI , Fatema JAGOT , Sydney NAMAUMBO , Noel Jabesi KAPITO , Deborah Charles TSUKULUZA , Loti BOTHA , Patrick NDOVIE , Patsani KUMAMBALA

Background

Selenium is an essential trace element that exists in various forms, including methylated species, each with distinct biological activities and toxicity profiles. Understanding these transformations is critical for evaluating selenium's role in health and the environment. This review was conducted through a targeted search of multiple databases, including PubMed, Scopus, Web of Science, and Google Scholar. Keywords such as "selenium methylation detection" and "analytical methods for selenium" were used to gather a broad and relevant selection of articles. Studies were included based on their relevance, methodological quality, and contributions to the field.

Results

The review provides a detailed analysis of both established and emerging analytical techniques for selenium detection. This includes gas chromatography-mass spectrometry (GC–MS), liquid chromatography-mass spectrometry (LC-MS), high-performance liquid chromatography (HPLC), X-ray absorption spectroscopy (XAS), and nuclear magnetic resonance (NMR). It evaluates the effectiveness of these methods in separating, identifying, and quantifying selenium species, with a particular focus on sensitivity, selectivity, and throughput. Additionally, new technologies such as capillary electrophoresis coupled with inductively coupled plasma-mass spectrometry (CE-ICP-MS) and laser-induced breakdown spectroscopy (LIBS) are discussed for their potential to enhance precision and efficiency.

Significance

This review highlights the critical role of advanced analytical methods in understanding selenium transformations and improving measurement accuracy. By addressing challenges such as matrix effects, overlapping retention times, and spectral interferences, the review underscores the importance of reliable selenium analysis for health and environmental assessments, and provides insights into the ongoing advancements in analytical technology.

硒是一种必需的微量元素，以多种形式存在，包括甲基化的形式，每种形式都具有不同的生物活性和毒性特征。了解这些转化对于评估硒在健康和环境中的作用至关重要。本综述是通过多个数据库的目标搜索进行的，包括PubMed、Scopus、Web of Science和谷歌Scholar。关键词如“硒甲基化检测”和“硒的分析方法”收集广泛和相关的文章选择。研究根据其相关性、方法质量和对该领域的贡献被纳入。结果对现有的和新兴的硒检测技术进行了详细的分析。这包括气相色谱-质谱（GC-MS），液相色谱-质谱（LC-MS），高效液相色谱（HPLC）， x射线吸收光谱（XAS）和核磁共振（NMR）。它评估了这些方法在分离、鉴定和定量硒的有效性，特别关注灵敏度、选择性和通量。此外，还讨论了毛细管电泳耦合电感耦合等离子体质谱（CE-ICP-MS）和激光诱导击穿光谱（LIBS）等新技术在提高精度和效率方面的潜力。本文综述了先进的分析方法在理解硒转化和提高测量精度方面的重要作用。通过解决诸如基质效应、重叠保留时间和光谱干扰等挑战，该综述强调了可靠的硒分析对健康和环境评估的重要性，并为分析技术的持续进步提供了见解。

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引用次数: 0

Analysis of metal electrochemical corrosion behavior and velocity under AC stray current 交流杂散电流作用下金属的电化学腐蚀行为及腐蚀速度分析

IF 1.2 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-03-29 DOI: 10.1016/j.cjac.2025.100528

Jianli LI, Jun AN, Haining YU, Jing WANG

Stray currents can cause electrochemical corrosion of metals, accelerate material aging, and even pose safety hazards. By studying corrosion behavior and speed, the degree of damage caused by stray currents to metals can be evaluated, protective measures (cathodic protection, insulation design, etc.) can be optimized, the service life of metal structures can be extended, maintenance costs can be reduced, and the safe and stable operation of power systems and infrastructure can be ensured. Therefore, research on the electrochemical corrosion behavior and velocity analysis method of metals under AC stray current. This article mainly explores the influence of different alternating current (AC) stray current densities on the electrochemical corrosion behavior of 316L stainless steel. The experiment used Yingtan soil simulation solution, and analyzed the changes in indicators through electrochemical testing, corrosion morphology observation, and corrosion rate calculation. The results indicate that the corrosion rate of 316L stainless steel in soil simulation solution shows a trend of first decreasing and then increasing when disturbed by AC stray current density. In the initial stage, the synergistic effect of high concentrations of Cl^– and O₂ leads to a faster corrosion rate. Over time, corrosion products increase and form a film layer, which hinders harmful ion erosion and slows down the corrosion rate. However, after prolonged immersion, the corrosion product film may crack, crevice, or even peel off, causing crevice corrosion and galvanic corrosion, accelerating the corrosion process. AC stray current forms a "tip discharge" through the defect, further exacerbating corrosion. With the increase of AC interference current density, the corrosion rate of 316L stainless steel significantly increases, and the main corrosion form changes from uniform corrosion to localized corrosion. When the stray current density is greater than or equal to 200 A/m², the corrosion degree of 316L stainless steel under the peeling coating reaches severe corrosion. This study is of great significance for understanding the impact of AC stray currents on metal corrosion and developing effective protective measures.

杂散电流会引起金属的电化学腐蚀，加速材料老化，甚至造成安全隐患。通过研究腐蚀行为和腐蚀速度，可以评估杂散电流对金属的破坏程度，优化保护措施（阴极保护、绝缘设计等），延长金属结构的使用寿命，降低维护成本，保证电力系统和基础设施的安全稳定运行。因此，研究了金属在交流杂散电流作用下的电化学腐蚀行为及速度分析方法。本文主要研究了不同交流杂散电流密度对316L不锈钢电化学腐蚀行为的影响。实验采用鹰潭土壤模拟溶液，通过电化学测试、腐蚀形态观察、腐蚀速率计算等分析指标变化。结果表明：受交流杂散电流密度干扰时，316L不锈钢在土壤模拟溶液中的腐蚀速率呈现先减小后增大的趋势；在初始阶段，高浓度Cl -和O2的协同作用导致腐蚀速率加快。随着时间的推移，腐蚀产物增加并形成膜层，阻止有害离子的侵蚀，减缓腐蚀速度。但在长时间浸泡后，腐蚀产品膜可能出现裂纹、裂缝，甚至剥落，引起缝隙腐蚀和电偶腐蚀，加速腐蚀过程。交流杂散电流通过缺陷形成“尖端放电”，进一步加剧腐蚀。随着交流干扰电流密度的增大，316L不锈钢的腐蚀速率显著增大，主要腐蚀形式由均匀腐蚀转变为局部腐蚀。杂散电流密度大于等于200 A/m2时，剥落涂层下的316L不锈钢腐蚀程度达到严重腐蚀。该研究对了解交流杂散电流对金属腐蚀的影响，制定有效的防护措施具有重要意义。

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引用次数: 0

Electrochemical surface modification and regeneration of carbon fiber microelectrodes in deionized water 碳纤维微电极在去离子水中的电化学表面改性与再生

IF 1.2 4区化学 Q4 CHEMISTRY, ANALYTICAL

Chinese Journal of Analytical Chemistry

Pub Date : 2025-03-25 DOI: 10.1016/j.cjac.2025.100531

Tao FANG , Tingting WANG , Uchkun ISHIMOV , Yuan LI , Ghulam MURTAZA , Awais IHSAN , Yanbing PAN , Ruiting TIAN , Han CHENG , Xianju HUANG

The contamination, passivation, or fouling of the detection electrodes is a serious problem undermining the analytical performance of electroanalytical devices. In this paper, a simple and effective carbon fiber microelectrodes (CFME) renewal method was proposed for the first time. CFME was pretreated with an initial potential of 1.75 V in deionized water for 26.13 min to obtain an activated electrode with a significantly increased electrochemical response to dopamine. This method can restore the electrochemical performance of the inactivated CFME. An advantage of this method is that its activation and regeneration effect on the electrode was not less than the other reported activation solutions, although deionized water does not contain any other electrolyte. Our study furthered the understanding of the activation mechanism of CFME treated electrochemically in deionized water, this was ascribed to a renewing in the surface of carbon fibers after electrochemical treatment. At the same time, it was proved that the oxygen-containing functional groups were modified on the surface of activated CFME, which led to the regeneration of an electrochemically active surface and improved CFME sensitivity. The differential pulse voltammetry (DPV) response of dopamine showed good linearity (R² = 0.9961) on the regenerated CFME in the concentration range from 1.0 × 10⁻⁷ to 1.0 × 10⁻⁴ mol/L. A limit of detection as low as 3.1 × 10^–8 mol/L was found. The regenerated CFME was quite stable and had good reproducibility. It is expected to be applied to activate and regenerate electrodes contaminated in the monitoring of a complex biological microenvironment.

检测电极的污染、钝化或污垢是一个严重的问题，会破坏电分析设备的分析性能。本文首次提出了一种简单有效的碳纤维微电极（CFME）更新方法。CFME在去离子水中以1.75 V的初始电位预处理26.13 min，得到对多巴胺电化学反应显著增强的活化电极。该方法可以恢复失活CFME的电化学性能。该方法的一个优点是，尽管去离子水不含任何其他电解质，但其对电极的激活和再生效果不低于其他报道的激活溶液。我们的研究进一步了解了CFME在去离子水中电化学处理后的活化机理，这归因于电化学处理后碳纤维表面的更新。同时证明了在活化的CFME表面修饰含氧官能团，使CFME的电化学活性表面再生，提高了CFME的灵敏度。在1.0 × 10−7 ~ 1.0 × 10−4 mol/L范围内，多巴胺对再生CFME的差分脉冲伏安（DPV）响应呈良好的线性关系（R2 = 0.9961）。检出限低至3.1 × 10-8 mol/L。再生CFME稳定性好，重现性好。它有望应用于复杂生物微环境监测中被污染的电极的激活和再生。

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引用次数: 0