Analytical Sciences最新文献

英文中文

Exploring the synchronized effect of MWCNT/X-manganate (X-Cu, Zn) nanocomposite for the sensitive and selective electrochemical detection of Hg(II) and Pb(II) in water 探索 MWCNT/X-锰酸盐（X-铜、锌）纳米复合材料在灵敏和选择性电化学检测水中汞（II）和铅（II）方面的同步效应。

IF 1.8 4区化学 Q3 CHEMISTRY, ANALYTICAL

Analytical Sciences

Pub Date : 2024-08-30 DOI: 10.1007/s44211-024-00652-1

Xingpu Qi, Ping Liu, Fang Yao, Mengli Zhao, Xuanyu Shen, Zhengyun Wang

The presence of heavy metal ions in the environment is a long-lasting problem that requires the simultaneous detection of Hg(II) and Pb(II) which is both vital and challenging. This present study examines a simplified and effective approach for synthesizing multi-walled carbon nanotube–copper manganese oxide (MWCNT–CuMn₂O₄) and multi-walled carbon nanotube–zinc manganese oxide (MWCNT–ZnMn₂O₄) nanocomposites for electrochemical detection of heavy metal ions. The nanocomposites MWCNT–CuMn₂O₄ and MWCNT–ZnMn₂O₄ exceptional electrochemical performance was evaluated using Square Wave Anodic Stripping Voltammetry (SWASV). The fabricated MWCNT–ZnMn₂O₄ demonstrated lower values of Electrochemical Impedance Spectroscopy (EIS) with charge transfer resistance (R_ct) of approximately 34.13 Ω. Remarkably, the MWCNT–ZnMn₂O₄ electrochemical sensor exhibited the widest linear ranges of 0.5–10 μM with sensitive detection limits (0.011 μM for Hg(II) and 0.014 μM for Pb(II)). Interestingly, the MWCNT–ZnMn₂O₄ sensor showed excellent capability in detecting Hg(II) and Pb(II) in real water samples with a recovery percentage of 94.1% and 91.3%. Overall, the MWCNT–ZnMn₂O₄ modified GCE showcased superior selectivity, sensitivity, reproducibility, stability, and repeatability.

Graphical abstract

环境中重金属离子的存在是一个长期存在的问题，需要同时检测汞（II）和铅（II），这既重要又具有挑战性。本研究探讨了一种合成多壁碳纳米管-铜锰氧化物（MWCNT-CuMn2O4）和多壁碳纳米管-锌锰氧化物（MWCNT-ZnMn2O4）纳米复合材料用于重金属离子电化学检测的简化而有效的方法。使用方波阳极剥离伏安法（SWASV）对纳米复合材料 MWCNT-CuMn2O4 和 MWCNT-ZnMn2O4 的优异电化学性能进行了评估。制备的 MWCNT-ZnMn2O4 的电化学阻抗谱（EIS）值较低，电荷转移电阻（Rct）约为 34.13 Ω。值得注意的是，MWCNT-ZnMn2O4 电化学传感器表现出最宽的线性范围（0.5-10 μM）和灵敏的检测限（汞（II）为 0.011 μM，铅（II）为 0.014 μM）。有趣的是，MWCNT-ZnMn2O4 传感器在实际水样中检测汞（II）和铅（II）的能力非常出色，回收率分别为 94.1%和 91.3%。总体而言，MWCNT-ZnMn2O4 改性 GCE 展示了卓越的选择性、灵敏度、再现性、稳定性和重复性。

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引用次数: 0

Recent technical development for on-site analysis 现场分析的最新技术发展。

IF 1.8 4区化学 Q3 CHEMISTRY, ANALYTICAL

Analytical Sciences

Pub Date : 2024-08-29 DOI: 10.1007/s44211-024-00628-1

Mao Fukuyama

引用次数: 0

Comparative study of machine-and deep-learning based classification algorithms for biomedical Raman spectroscopy (RS): case study of RS based pathogenic microbe identification 基于机器和深度学习的生物医学拉曼光谱（RS）分类算法比较研究：基于 RS 的病原微生物识别案例研究。

IF 1.8 4区化学 Q3 CHEMISTRY, ANALYTICAL

Analytical Sciences

Pub Date : 2024-08-29 DOI: 10.1007/s44211-024-00645-0

Sisi Guo, Ruoyu Zhang, Tao Wang, Jianfeng Wang

One key aspect pushing the frontiers of biomedical RS is dedicated machine- or deep- learning (ML or DL) algorithms. Yet, systematic comparative study between ML and DL algorithms has not been conducted for biomedical RS, largely due to the limited availability of open-source and large Raman spectra dataset. Therefore we compared typical ML partial least square-discriminant analysis (PLS-DA) and DL one dimensional convolution neural network (1D-CNN) based pathogenic microbe identification on 12,000 Raman spectra from six species of microbe (i.e., K. aerogenes (Klebsiella aerogenes), C. albicans (Candida albicans), C. glabrata (Candida glabrata), Group A Strep. (Group A Streptococcus), E. coli1 (Escherichia coli1), E. coli2 (Escherichia coli2)) when 100%, 75%, 50% and 25% of the 12,000 Raman spectra were retained. The total Raman dataset was analyzed with 80% split for training and 20% for testing. The 100% retained testing dataset accuracy, area under curve (AUC) of the receiver operating characteristic (ROC) curve were 95.25% and 0.997 for 1D-CNN, which are higher than those (89.42% and 0.979) of PLS-DA. Yet, PLS-DA outperforms 1D-CNN for 75%, 50% and 25% retained testing dataset. The resultant accuracies and AUCs demonstrated the performance reliance of PLS-DA and 1D-CNN on Raman spectra number. Besides, both loadings on the latent variables of PLS-DA and the saliency maps of 1D-CNN largely captured Raman peaks arising from DNA and proteins with comparable interpretability. The results of the current work indicated that both ML and DL algorithms should be explored for application-wise Raman spectra identification to select whichever with higher accuracies and AUCs.

Graphical abstract

推动生物医学 RS 前沿发展的一个关键方面是专用机器学习或深度学习（ML 或 DL）算法。然而，由于开源的大型拉曼光谱数据集有限，尚未对生物医学 RS 的 ML 算法和 DL 算法进行系统的比较研究。因此，我们比较了基于 ML 偏最小二乘法判别分析（PLS-DA）和 DL 一维卷积神经网络（1D-CNN）的典型病原微生物识别方法，对来自六种微生物（即、A组链球菌）、大肠杆菌1（Escherichia coli1）、大肠杆菌2（Escherichia coli2））的 12,000 拉曼光谱进行病原微生物鉴定。对拉曼数据集进行了分析，其中 80% 用于训练，20% 用于测试。1D-CNN 100%保留测试数据集的准确率和接收者操作特征曲线（ROC）下面积（AUC）分别为 95.25% 和 0.997，高于 PLS-DA 的准确率和接收者操作特征曲线下面积（AUC）（89.42% 和 0.979）。然而，在保留 75%、50% 和 25% 的测试数据集中，PLS-DA 的结果优于 1D-CNN 的结果。由此得出的精确度和 AUC 值表明，PLS-DA 和 1D-CNN 的性能依赖于拉曼光谱数。此外，PLS-DA 的潜在变量负载和 1D-CNN 的显著性图谱在很大程度上都捕捉到了 DNA 和蛋白质产生的拉曼峰，其可解释性相当。本次研究的结果表明，在拉曼光谱的应用识别中，应同时探索 ML 算法和 DL 算法，以选择准确率和 AUC 较高的算法。

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引用次数: 0

Aptamer regulated peroxidase-like activity of cobalt oxyhydroxide nanosheets for colorimetric detection of kanamycin 用于卡那霉素比色检测的氢氧化钴纳米薄片的过氧化物酶样活性受色素调节。

IF 1.8 4区化学 Q3 CHEMISTRY, ANALYTICAL

Analytical Sciences

Pub Date : 2024-08-28 DOI: 10.1007/s44211-024-00655-y

Shuyan Xiao, Jiafeng Wu, Mingqin Kang, Zhongping Dong

A straightforward label-free colorimetric aptasensor utilizing the aptamer-enhanced peroxidase-like activity of cobalt oxyhydroxide (CoOOH) nanosheets has been established for kanamycin detection. In the kanamycin-free state, aptamers adsorb onto the CoOOH surface through electrostatic forces, enhancing the peroxidase-like activity of CoOOH and thereby resulting in a strong absorption signal and a yellow hue in 3,3′,5,5′-tetramethylbenzidine (TMB) upon termination of the reaction with a stop solution. Conversely, upon the introduction of kanamycin, aptamers and CoOOH nanosheets compete for binding to kanamycin, resulting in a significant decrease in the number of aptamers bound to CoOOH. As a result, the activity of CoOOH diminishes, leading to a corresponding reduction in coloration and absorbance of the solution. Hence, the quantitative determination of kanamycin could be realized by analyzing the absorbance variations. Under optimal conditions, the aptasensor demonstrated high sensitivity and specificity, with a linear detection range from 500 nM to 5 µM and a detection limit as low as 54.6 nM. Moreover, the aptasensor effectively identified kanamycin in river water samples, achieving a recovery rate between 91.7% and 102.1%. This approach offers good practicability and provides a novel platform for kanamycin detection in environmental samples.

Graphical abstract

利用纳米氧化钴（CoOOOH）的合体增强过氧化物酶样活性，建立了一种直接的无标记比色合体传感器，用于检测卡那霉素。在不含卡那霉素的状态下，适配体通过静电力吸附在 CoOOH 表面，增强了 CoOOH 的过氧化物酶样活性，因此在用停止液终止反应后，3,3',5,5'-四甲基联苯胺（TMB）会产生强烈的吸收信号和黄色色调。相反，引入卡那霉素后，适配体和 CoOOH 纳米片会竞争性地与卡那霉素结合，导致与 CoOOH 结合的适配体数量显著减少。因此，CoOOH 的活性降低，导致溶液的着色和吸光度也相应降低。因此，可以通过分析吸光度的变化来实现卡那霉素的定量测定。在最佳条件下，该灵敏度和特异性都很高，线性检测范围为 500 nM 至 5 µM，检测限低至 54.6 nM。此外，该灵敏传感器还能有效鉴定河水样本中的卡那霉素，回收率在 91.7% 到 102.1% 之间。该方法具有良好的实用性，为环境样品中卡那霉素的检测提供了一个新平台。

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引用次数: 0

Removal of ceftriaxone and cefotaxime antibiotics from industrial wastewater via complexation with Cu(II) 通过与铜（II）络合去除工业废水中的头孢曲松和头孢噻肟抗生素。

IF 1.8 4区化学 Q3 CHEMISTRY, ANALYTICAL

Analytical Sciences

Pub Date : 2024-08-25 DOI: 10.1007/s44211-024-00632-5

Doaa A. Abdel-Kader, Adel M. Kamal Eldean, Mohamed M. Abd El-Wahab, Mohamed S. Galal, Elham Y. Hashem

A high-performance liquid chromatographic method (HPLC) with UV detection is described for determination of ceftriaxone sodium (CFX) and cefotaxime sodium (CFM) content in pharmaceutical industrial wastewater. These methods are based on the detection of these antibiotics via the formation of chelate complexes with Cu(II). The developed Liquid Chromatographic method offers symmetric peak shape, good resolution and reasonable retention time for both drugs. The removal percentage reached about 100 and 92.1% at pH 7.2 for CFX and CFM, respectively. In UV detection, the removal of the chelating antibiotics were based on forming of chelate complexes with Cu(II) which detected at λ_{max =} 253 and 244 nm for CFX and CFM, respectively. Linearity, accuracy and precision were found to be acceptable over the concentration range of 5.99–59.86 µg mL⁻¹ for CFX and 14.33–71.63 µg mL⁻¹ for CFM. The proposed method can be used for the quality control of industrial wastewater containing CFX and CFM.

Graphical abstract

介绍了一种高效液相色谱法（HPLC）和紫外检测法，用于测定制药工业废水中头孢曲松钠（CFX）和头孢噻肟钠（CFM）的含量。这些方法通过与 Cu(II) 形成螯合物来检测这些抗生素。所开发的液相色谱法对这两种药物具有对称的峰形、良好的分辨率和合理的保留时间。在 pH 值为 7.2 时，CFX 和 CFM 的去除率分别达到约 100%和 92.1%。在紫外检测中，螯合抗生素的去除是基于与 Cu(II) 形成的螯合物，CFX 和 CFM 的检测波长分别为 λmax = 253 nm 和 244 nm。结果表明，在 CFX 5.99-59.86 µg mL-1 和 CFM 14.33-71.63 µg mL-1 的浓度范围内，线性关系、准确度和精密度均可接受。该方法可用于含有 CFX 和 CFM 的工业废水的质量控制。

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引用次数: 0

SERS detection of uranyl based on MOF-coated gold nanooctahedron hybrid 基于 MOF 涂层金纳米八面体杂化物的 SERS 检测铀酰。

IF 1.8 4区化学 Q3 CHEMISTRY, ANALYTICAL

Analytical Sciences

Pub Date : 2024-08-24 DOI: 10.1007/s44211-024-00646-z

Chao Yuan, Hongwei Ge, Benmei Cao, Suhua Wang

The ability to sensitively and quantitatively detect uranyl in complex samples plays a vital role in environmental monitoring. In this work, an MOF-coated gold (Au) nanohybrid was synthesized for uranyl detection by surface-enhanced Raman scattering (SERS) technology. The MOF shell not only prevents the Au nanoparticles from rapid aggregation, but also effectively enhances the Raman signal of uranyl. A detection limit of as low as 0.5 μM could be achieved in solution, which could be comparable to the previously reported ones from SERS-based approaches. Moreover, the prepared SERS-active substrate was also applied to uranyl detection in real samples.

Graphical Abstract

能够灵敏、定量地检测复杂样品中的铀酰在环境监测中起着至关重要的作用。本研究利用表面增强拉曼散射（SERS）技术合成了一种 MOF 涂层金（Au）纳米杂化物，用于检测铀酰。MOF 外壳不仅能防止金纳米粒子快速聚集，还能有效增强铀酰的拉曼信号。溶液中的检测限低至 0.5 μM，与之前报道的基于 SERS 方法的检测限相当。此外，制备的 SERS 活性基底还被应用于实际样品中的铀酰检测。

引用次数: 0

Correction: New stability indicating RP-HPLC methods for the determination of related substances and assay of trametinib acetic acid: a mass balance approach 更正：用于测定相关物质和检测曲美替尼乙酸的新型稳定性指示 RP-HPLC 方法：质量平衡法。

IF 1.8 4区化学 Q3 CHEMISTRY, ANALYTICAL

Analytical Sciences

Pub Date : 2024-08-21 DOI: 10.1007/s44211-024-00650-3

G. Himabindu, Y. Satyanarayana Reddy, A. V. S. S. Prasad, C. Ramadas, Hemant Kumar Sharma

引用次数: 0

Combination of on-line sample preconcentration by large-volume dual preconcentration by isotachophoresis and stacking (LDIS) with field-amplified sample injection (FASI) on Y-channel microchips 在 Y 型通道微芯片上将大容量异向电泳和堆积双重预浓缩（LDIS）在线样品预浓缩与现场放大样品进样（FASI）相结合。

IF 1.8 4区化学 Q3 CHEMISTRY, ANALYTICAL

Analytical Sciences

Pub Date : 2024-08-20 DOI: 10.1007/s44211-024-00647-y

Fumihiko Kitagawa, Sora Sato, Tomohiro Suzuki, Takayuki Kawai

In our previous study, the combination of two on-line sample preconcentration techniques, large-volume sample stacking with an electroosmotic flow (EOF) pump (LVSEP) and transient isotachophoresis (tITP), in microchip electrophoresis (MCE) was developed, which was named large-volume dual preconcentration by isotachophoresis and stacking (LDIS). LDIS was apparently effective for improving the sensitivity and the peak shape. In LDIS, however, there was a limit to the improvement of the sensitivity enhancement factor (SEF) since the amount of analytes to be concentrated was limited to the channel volume. To overcome this issue, in the present article, LDIS was coupled with field-amplified sample injection (FASI) technique on Y-shaped channel microchips. The use of a Y-channel in LDIS-FASI allowed consecutive LVSEP, FASI and tITP enrichments with a simple voltage control. In conventional LVSEP and LDIS analyses of a standard analyte, the SEFs were evaluated to be 2630 and 13,100, respectively, whereas in LDIS-FASI that was increased to 27,900 even at the FASI injection time of 0 s. To achieve higher SEFs, furthermore, the FASI injection time was increased to 150 s, resulting in the best SEF of 58,500. It should be emphasized that the peak width in LDIS-FASI was quite narrow, only 0.3–3.1 s, while in normal LVSEP that was 13 s. Furthermore, the LDIS-FASI technique was applied to the analysis of oligosaccharide mixture. Due to the focusing effect by LDIS-FASI, the resolutions were improved from 0.97–1.57 to 2.08–2.73.

Graphical Abstract

我们在之前的研究中开发了微芯片电泳（MCE）中两种在线样品预浓缩技术的组合，即使用电渗流（EOF）泵的大容量样品堆积（LVSEP）和瞬时等渗电泳（tITP），并将其命名为大容量等渗电泳和堆积双重预浓缩（LDIS）。LDIS 在提高灵敏度和改善峰形方面效果明显。然而，在 LDIS 中，灵敏度增强因子（SEF）的提高是有限度的，因为需要浓缩的分析物的量受限于通道体积。为了克服这一问题，本文将 LDIS 与 Y 型通道微芯片上的场放大样品进样（FASI）技术相结合。在 LDIS-FASI 中使用 Y 型通道，只需简单的电压控制就能实现连续的 LVSEP、FASI 和 tITP 富集。在对标准分析物进行传统的 LVSEP 和 LDIS 分析时，SEF 分别为 2630 和 13100，而在 LDIS-FASI 中，即使 FASI 注入时间为 0 秒，SEF 也增至 27900。需要强调的是，LDIS-FASI 的峰宽非常窄，只有 0.3-3.1 秒，而普通 LVSEP 的峰宽为 13 秒。由于 LDIS-FASI 的聚焦效应，分辨率从 0.97-1.57 提高到 2.08-2.73。

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引用次数: 0

Enzyme-aided amplification strategy for sensitive detection of methamphetamine based on fluorescence aptamer sensor 基于荧光适配体传感器灵敏检测甲基苯丙胺的酶辅助放大策略。

IF 1.8 4区化学 Q3 CHEMISTRY, ANALYTICAL

Analytical Sciences

Pub Date : 2024-08-16 DOI: 10.1007/s44211-024-00648-x

Zheyu Wang, Yandan Wang, Yishuo Tong, Weifen Niu

Methamphetamine (METH) abuse poses a serious risk to human health and social stability. It is critical to develop sensitive and selective methods for detecting METH. Here, we develop a fluorescence aptamer sensor to detect METH based on DNA exonuclease III (Exo III), graphene oxide (GO), and FAM-labeled aptamer. First, the sensor used GO’s strong binding capacity to adsorb and quench the fluorescence of the aptamer attached to GO surface. When METH was added to the system, the formation of stable complex for aptamer and METH dissociated from the surface of GO, leading to a fluorescence restoration. Then, the fluorescence signal was further amplified by using Exo III to liberate target METH for cyclic hybridization. And the gel electrophoresis experiment further verified the reliability of this strategy. This aptamer sensor exhibited a low detection limit (0.52 nM) and excellent selectivity under optimal conditions. Notably, this sensor has been successfully validated in the detection of METH in urine and saliva samples, exhibited commendable recovery (94.00–104.65%). Its benefits include facile, sensitive, and rapid. Expected to be used in practical METH detection.

Graphical abstract

甲基苯丙胺（METH）滥用对人类健康和社会稳定构成严重威胁。开发灵敏且具有选择性的甲基苯丙胺检测方法至关重要。在此，我们以 DNA 外切酶 III（Exo III）、氧化石墨烯（GO）和 FAM 标记的适配体为基础，开发了一种检测 METH 的荧光适配体传感器。首先，该传感器利用 GO 的强结合能力吸附并淬灭附着在 GO 表面的适配体的荧光。当向系统中加入 METH 时，贴体与 METH 形成的稳定复合物从 GO 表面解离，从而恢复荧光。然后，利用 Exo III 进一步放大荧光信号，释放出目标 METH 进行循环杂交。凝胶电泳实验进一步验证了这一策略的可靠性。在最佳条件下，该传感器的检测限低（0.52 nM），选择性好。值得注意的是，该传感器已成功用于检测尿液和唾液样本中的甲基苯丙胺，回收率高达 94.00-104.65%。其优点包括简便、灵敏和快速。有望用于实际的 METH 检测。

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引用次数: 0

Separation of iodate, bromide, nitrite, nitrate, and iodide in seawater by ion chromatography using 1-aminoundecyl group chemically bonded silica columns 利用 1-aminoundecyl 基团化学键合硅胶柱，通过离子色谱法分离海水中的碘酸根、溴化物、亚硝酸盐、硝酸盐和碘化物。

IF 1.8 4区化学 Q3 CHEMISTRY, ANALYTICAL

Analytical Sciences

Pub Date : 2024-08-14 DOI: 10.1007/s44211-024-00639-y

Kazuaki Ito, Michinari Noguchi, Yuuta Horioka, Joji Ohshita, Takeshi Hirokawa

The separation and detection of six common inorganic anions (iodate (IO₃⁻), bromate (BrO₃⁻), bromide (Br⁻), nitrite (NO₂⁻), nitrate (NO₃⁻), and iodide (I⁻)) in pure water and 35 ‰ artificial seawater were examined by ion chromatography (IC). As packing materials of separation columns, 1-aminoundecyl group chemically bonded silica (AUS) gels were prepared. Separation of the anions in pure water was achieved using separation columns (150 mm × 4.6 mm i.d.) packed with the AUS gels, 0.1 M NaCl + 5 mM phosphate buffer (pH 4.5) as eluent, and a UV detector (wavelength 225 nm). The anions in artificial seawater were separated and detected with a 300 mm-long column without interferences by matrix anions such as chloride (Cl⁻) and sulfate (SO₄²⁻). The stationary phases have high-capacity anion-exchange/hydrophilic/hydrophobic interaction mixed-modes. The IC system was applied to five inorganic anions, IO₃⁻, Br⁻, NO₂⁻, NO₃⁻, and I⁻ in seawater of the Seto-Inland Sea, Japan. The detection limits (DLs, S/N = 3) were 11 µg L⁻¹ (IO₃⁻), 93 (Br⁻), 1.3 (NO₂⁻), 1.4 (NO₃⁻), and 1.1 (I⁻) for a 100-µL sample injection.

Graphical abstract

利用离子色谱法（IC）研究了纯水和 35 ‰ 人工海水中六种常见无机阴离子（碘酸根（IO3-）、溴酸根（BrO3-）、溴化物（Br-）、亚硝酸根（NO2-）、硝酸根（NO3-）和碘化物（I-））的分离和检测。作为分离柱的填料，制备了 1-aminoundecyl 基团化学键合二氧化硅（AUS）凝胶。使用以 AUS 凝胶、0.1 M NaCl + 5 mM 磷酸盐缓冲液（pH 4.5）为洗脱剂的分离柱（150 mm × 4.6 mm i.d.）和紫外检测器（波长 225 nm）分离纯水中的阴离子。使用 300 毫米长的色谱柱分离和检测人工海水中的阴离子，不会受到氯离子（Cl-）和硫酸根离子（SO42-）等基质阴离子的干扰。固定相具有高容量阴离子交换/亲水/疏水相互作用混合模式。该 IC 系统被应用于日本濑户内海海水中的 IO3-、Br-、NO2-、NO3- 和 I- 五种无机阴离子。注入 100µL 样品的检测限（DLs，S/N = 3）分别为 11 µg L-1（IO3-）、93（Br-）、1.3（NO2-）、1.4（NO3-）和 1.1（I-）。

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