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SPECTROCHIMICA ACTA PART B-ATOMIC SPECTROSCOPY · 2025 · IF 3.8

High-sensitivity quantification of Tilletia foetida teliospores in wheat via immunomagnetic enrichment and gold nanoparticle-labeled ICP-MS immunoassay

Yufeng Li,Hanxu Ji,Jingjing Xu,Xiuming Mei,Xiaoxiao Wu,Yongli Ye,Miao Yang,Diyao Jiang,Yuwei Qiang,Lan Jiang,Jungui Zhou,Chi Zhang,Xiulan Sun

A novel method for detecting Tilletia foetida teliospores in wheat was developed by integrating inductively coupled plasma mass spectrometry (ICP-MS) with an elemental labeling strategy. On the basis of an immunological method, capture magnetic beads coupled with a polyclonal antibody probe (MBs-pAb) were constructed to specifically enrich and label T. foetida teliospores. A gold nanoparticle-labeled monoclonal antibody was then added to bind to MBs-pAb. After dissociation of the resulting complexes using citric acid, the 197 Au signal was detected by ICP-MS, allowing for the quantitative detection of T. foetida spores. Under optimal conditions, the method had a limit of detection of 50 teliospores/mL and a linear range of 200–50,000 teliospores/mL. This new approach, which enables the rapid and highly sensitive detection of teliospores within 2.5 h, was successfully applied to wheat samples. The method shows significant potential for analyzing and monitoring common bunt of wheat, offering a robust tool for agricultural diagnostics and disease management.

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GEOSTANDARDS AND GEOANALYTICAL RESEARCH · 2024 · IF 2.7

Tourmaline Megacryst Reference Materials for High Precision In Situ Boron Isotope and Elemental Measurement by LA-MC-ICP-MS

Xiuhong Liao,Tao Chen,Tao Luo,Yue Cai,Wen Zhang,Zuowei Yin,Zhaochu Hu

Tourmaline serves as a vital recorder of geological processes. However, suitable tourmaline reference materials (RMs) for elemental and stable isotopic composition in situ measurements are still limited. In this study, three tourmaline megacrysts (MD-B66, IM-B232 and BR-DG68) were characterised as potential RMs for B isotope measurements by LA-MC-ICP-MS and mass fraction determinations by LA-ICP-MS. Over 251 measurements with LA-MC-ICP-MS on ten randomly selected fragments from MD-B66 consistently yielded B isotope ratios of -7.74 ± 0.25‰ (2 s ), establishing MD-B66 as a suitably homogeneous primary reference material for high-precision, in situ microbeam B isotope measurements. Notably, the (long-term) intermediate precision of 0.25‰ (2 s ) for in situ B isotope measurements obtained using this reference material is comparable to that reported from solution MC-ICP-MS methods in the literature. Two other tourmaline megacrysts, with intermediate precision ranging from ± 0.48‰ to ± 0.61‰ (2 s ) for δ 11 B measurement, can be employed as secondary RMs for quality control. The mean δ 11 B values determined by solution MC-ICP-MS for MD-B66 (-7.71 ± 0.32‰, n = 12), IM-B232 (-13.17 ± 0.62‰, n = 8) and BR-DG68 (-13.85 ± 0.32‰, n = 12), with expanded uncertainties at the 95% confidence level, are consistent with those determined by LA-MC-ICP-MS. Among these three new RMs, BR-DG68 displays relatively homogeneous major and trace element mass fractions. Characterisation using both in situ and wet chemical techniques demonstrated the suitability of BR-DG68 as the first tourmaline reference material for elemental measurement by LA-ICP-MS, which would permit matrix-matched and therefore more accurate elemental measurement in tourmalines. Unlike electron probe microanalysis with B and Li contents calculated based on stoichiometric assumptions, direct and accurate measurements of the two low atomic number elements, along with other major and trace elements can be achieved by LA-ICP-MS with the aid of the newly developed tourmaline reference material BR-DG68. Overall, current and future studies in geochemistry may benefit from these newly proposed tourmaline RMs, which should lead to significantly improved precision and accuracy for in situ B isotope and elemental measurement.

研究领域: 地质学 · 地球化学
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ANALYTICA CHIMICA ACTA · 2026 · IF 6.1

Measurement of Pb isotopes for geological samples by MC-ICP-MS coupled with an extraction resin column preconcentration method

Xin Li,Qiao-Hui Zhong,Jia-Kai Guo,Mei-Ju Li,Gao-Bin Chu,Jie Li

N235 extraction resin enables efficient Pb separation from geological reference materials. • Matrix are removed with dilute HBr and water, followed by Pb separation using low-concentration HBr. • The purified Pb is ready for MC-ICP-MS analysis without any evaporation step. • The method reliability is validated using various reference materials. • Pb isotope ratios of JA-1a are reported for the first time. Lead isotopic variations provide crucial insights into geochemical reservoirs, environmental sources, and geological ages. To obtain precise Pb isotope data by MC-ICP-MS, we develop a simple and efficient separation procedure using trialkyl amine (N235) resin. Batch experiments show that N235 strongly adsorbs Pb in 0.4 mol L −1 HBr, weakly in HCl, and not at all in HNO 3 media. Specifically, the optimized column procedure achieved high Pb recovery (94.5%) and eluted Pb in 0.5 mol L −1 HNO 3 , allowing direct measurement without evaporation, thereby reducing procedural blanks. The method was validated with ten reference materials (GSR-1, GSR-2, GSR-3, GSR-7, GSP-2, BHVO-2, JA-2, JG-2, JB-2, and JA-1a). Measured 206 Pb/ 204 Pb, 207 Pb/ 204 Pb and 208 Pb/ 204 Pb ratios agreed with published values within uncertainty, with external reproducibility better than 0.05% (RSD). Owing to its simplicity, high recovery, low blank, and low cost, this method offers a practical pretreatment strategy for high-precision Pb isotope analysis in diverse geological samples. A very simple, low-blank, and effective Pb purification method with a self-made trialkyl amine extraction resin is developed to separate Pb from geological reference materials for high precision determination of Pb isotopic compositions by MC-ICP-MS. Download: Download high-res image (254KB) Download: Download full-size image

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TALANTA · 2026 · IF 6.7

Automated analysis of ultra-trace 236U and natural uranium isotopes via integrated sample preparation and ICP-MS/MS detection

Jisheng Chen,Youyi Ni,Wenting Bu,Yue Luo,Bingjun Chen,Xuemei Liu,Chuting Yang,Junwen Wu,Hai Wang

Highly efficient and accurate analysis of ultra-trace anthropogenic 236 U in the presence of natural uranium isotopes is essential for nuclear forensics and environmental monitoring. In this study, we developed an integrated analytical method for the determination of 234 U, 235 U, 236 U, and 238 U by combining highly automated sample preparation with highly sensitive ICP-MS/MS detection. Automated total dissolution was employed to ensure complete extraction of both endogenous and exogenous uranium from solid matrices, while reproducible chemical separation was achieved using an automated platform equipped with regenerable UTEVA resin. This optimized procedure yielded exceptionally low operational blanks for 236 U at femtogram level. Moreover, the final eluent volume was minimized to 1.5 mL, allowing direct introduction into the ICP-MS/MS. By utilizing a membrane desolvation sample introduction system and a novel mass-shift mode (targeting UO 2 + species), the ICP-MS/MS sensitivity exceeded 4.1×10 6 cps/ppb, while the 235 UH + interference formation rate for 236 U was suppressed to 7.1×10 -10 . Consequently, the achieved detection limits for 236 U and the 236 U/ 238 U atom ratio were as low as 1.85 fg/g and 5×10 -12 , respectively. This method was successfully applied to determine the uranium isotopic composition in sediments from the adjacent sea area of the Daya Bay Nuclear Power Plant. These results demonstrate that the proposed method provides a robust and high-throughput solution for accurately quantifying of ultra-trace 236 U in environmental samples, such as those impacted by the global fallout.

CAS / MDL: 7601-90-3
✓ 已验证 产品关联 DOI PubMed 高影响因子
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NanoImpact · 2016 · IF 0

Determination of metal oxide nanoparticles and their ionic counterparts in environmental waters by size exclusion chromatography coupled to ICP-MS

Xiao-Xia Zhou,Jing-Fu Liu,Fang-Lan Geng

Analysis of metal oxide nanoparticles (MO NPs) and their released metal ions (M n+ ) is essential for understanding their environmental effects and biological toxicity. For the first time, size exclusion chromatography (SEC) was coupled with inductively coupled plasma mass spectrometry (ICP-MS) for speciation analysis of MO NPs and their corresponding M n+ . By using a 1000   Å poresize silica column, and an acetate buffer (pH   7.0, 10   mM) containing 10   mM sodium dodecyl sulfate (SDS) as a mobile phase at a flow rate of 0.5   mL/min, M n+ and MO NPs with sizes smaller than the column poresize were baseline separated within 10   min, whereas MO NPs with sizes larger than the exclusion limit were filtered off by the column. More importantly, this mobile phase is able to avoid the dissolution of MO NPs during the SEC separation. The high recoveries (>   97%) of M n+ from the SEC column ensured their accurate quantification directly with the online coupled SEC-ICP-MS, while the quantification of MO NPs by subtracting the M n+ content from the total metal content, which was determined with ICP-MS after digestion without SEC separation, efficiently eliminating the influence of retention of large MO NPs in the column. MO NPs with different sizes and compositions including NiO, CoO, ZnO, CuO and CeO 2 NPs were analyzed with this proposed method, with low detection limits (0.016–0.390   μg/L for both M n+ and MO NPs) and relative standard deviations (<   0.4% for retention time and <   2.2% for peak area at 50   μg/L M n+ ). The proposed method was verified by analyzing Ni 2+ , Ce 4+ , NiO and CeO 2 NPs in various environmental waters, with spiked recoveries in the range of 80.8–105.1%. Our method has great potential for speciation analysis of MO NPs and their corresponding M n+ in the environmental waters.

研究领域: 分析化学 · 环境科学
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JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY · 2020 ·Vol. 35 ·期 5 ·886-895 · IF 3.498

Development of REE-doped CaWO4 single crystals as reference materials for in situ microanalysis of scheelite via LA-ICP-MS

Yuqiu Ke,Jianzong Zhou,Xiaoqing Yi,Yijian Sun,Jianfeng Shao,Shiyong You,Wei Wang,Yunzhi Tang,Chaoyang Tu

Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been widely used for in situ microanalysis of elemental concentrations in solid samples, but its application is hampered by a lack of matrix-matched and homogeneous reference materials (RMs). In this work, a new method for preparing matrix-matched and homogeneous LA-ICP-MS reference materials has been developed. A multiple rare earth element (REE) doped CaWO4 single crystal (CaW-1) was successfully prepared by the Czochralski technique. The matrix composition and crystal structure were confirmed by X-ray diffraction (XRD) and electron microprobe analysis (EMPA), which indicates that these crystals have a matrix composition of CaWO4 and are matrix-matched with natural scheelite. The homogeneity of REE distribution was systematically studied by seven methods and the results demonstrated that REEs are distributed homogeneously in the CaWO4 single crystal with slight fluctuation (RSDs: ca. 4%). It can be concluded that the synthesized CaWO4 single crystal meets both crucial requirements, matrix-matched and homogeneous distribution, for an LA-ICP-MS reference material, and therefore it was used to quantitatively calibrate REE concentrations in natural scheelite. The results showed that acceptable analytical errors (<8%) were obtained, which were more desirable than those obtained with non-matrix-matched NIST SRM 610 as the RM. It robustly validates the ability of the developed method for preparing CaWO4 single crystals as possible LA-ICP-MS reference materials to calibrate REE concentrations in natural scheelite.

研究领域: 矿物学 · 分析化学
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ANALYTICAL LETTERS · 2024 · IF 1.6

Determination of Titanium (IV) Oxide Nanoparticles Released from Textiles by Single Particle – Inductively Coupled Plasma – Mass Spectrometry (SP-ICP-MS)

Chaoying Zhang,Qin Zhang,Yingchun Zhao,Dianquan Dong,Longjiang Huang

Monitoring TiO2 nanoparticles (NPs) that are released from functional textiles is significant for assessing the potential risk to consumers. However, determining the size distribution of TiO2 NPs is still a challenge due to agglomeration. The present study employed single particle–inductively coupled plasma–mass spectrometry (SP-ICP-MS) to quantify TiO2 NPs released from functional textiles. Through screening dispersants and validating the standard samples, an accurate method for determining the size and number of TiO2 NPs was developed. The validated procedure was successfully used to determine the release of TiO2 NPs from yarn in sweat and water media throughout the day. The result revealed that the yarn decorated with TiO2 NPs released approximately the same particle size distribution from 60 to 260 nm in both media. The released particle concentration was 0.094 µg/mL with a mean size of 136 nm in water and a particle concentration of 0.120 µg/mL with a mean size of 133 nm in sweat. Additionally, based upon transmission electron microscopy, anatase TiO2 NPs were identified. It is expected that this work is significant in the evaluation of the toxicological effects of multifunctional textiles modified by TiO2 NPs on human health.

研究领域: 环境科学 · 毒理学 · 纳米材料科学
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TALANTA · 2017 · IF 4.162

Gold nanoparticle labeling with tyramide signal amplification for highly sensitive detection of alpha fetoprotein in human serum by ICP-MS

Xiaoting Li,Beibei Chen,Man He,Guangyang Xiao,Bin Hu

In this work, we developed an immunoassay based on tyramide signal amplification (TSA) and gold nanoparticles (Au NPs) labeling for highly sensitive detection of alpha fetoprotein (AFP) by inductively coupled plasma mass spectrometry (ICP-MS). AFP was captured by anti-AFP1 coating on the 96-well plate and labeled by anti-AFP2-horseradish peroxidase (HRP), in which the HRP can catalyze the deposition of biotinylated tyramine on the nearby protein. Then the streptavidin (SA)-Au NPs was labeled on the deposited biotinylated tyramine as the intensive signal probe for ICP-MS measurement. Under the optimal experimental conditions, the limit of detection of the developed method for AFP was 1.85   pg/mL and the linear range was 0.005–2   ng/mL. The relative standard deviation for seven replicate detections of 0.01   ng/mL AFP was 5.2%. The proposed method was successfully applied to the detection of AFP in human serum with good recoveries. This strategy is highly sensitive and easy to operate, and can be extended to the sensitive detection of other biomolecules in human serum.

CAS / MDL: 9048-46-8 7697-37-2
研究领域: 分析化学 · 医学检验 · 纳米生物学
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TALANTA · 2018 · IF 4.244

Analysis of metallic nanoparticles and their ionic counterparts in complex matrix by reversed-phase liquid chromatography coupled to ICP-MS

Yuan Yang,Li Luo,Hai-Pu Li,Qiang Wang,Zhao-Guang Yang,Zhi-Peng Qu,Ru Ding

Developing quantification and characterization methodology for metallic nanoparticles (MNPs) and their ionic component in complex matrix are crucial for the evaluation of their environmental behavior and health risks to humans. In this study, reversed phase high performance liquid chromatography combined ICP-MS was established for the characterization of MNPs in complex matrix. The ionic component could be separated from NPs with the optimized parameters of aqueous mobile phase . Good linear relationship between average diameter and retention time of NPs was obtained using HPLC-ICP-MS and the size smaller than 40 nm could be determined with this method, the detected results were in accordance with TEM results. The low detection limit of AuNPs and Au(Ⅲ) (both in sub-μg/L level) showed that this method was promising for the characterization of AuNPs and Au(Ⅲ) in environmental water. The mass concentration of ionic Au(Ⅲ) in environmental water could be detected using the proposed HPLC-ICP-MS and the concentration of AuNPs was obtained by subtracting the Au(Ⅲ) concentration from the total Au (The concentration of total Au was detected by ICP-MS after microwave digestion). Furthermore this proposed HPLC-ICP-MS method and single particle-ICPMS (SP-ICP-MS) was used for the analysis of the Ag speciation in commercial antibacterial products.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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Jove-Journal of Visualized Experiments · 2021 · IF 1.355

Intracavernous Pressure Recording in a Cavernous Nerve Injury Rat Model

Zitaiyu Li,Yinghao Yin,Kancheng He,Kun Ye,Jun Zhou,Hao Qi,Yihong Zhou,Yingbo Dai,Yuxin Tang

The bilateral cavernous nerve (CN) injury rat model has been extensively used to simulate clinical cavernous nerve injury associated with erectile dysfunction (ED) for evaluating the effect of clinical therapeutic methods. However, the methods of CN injury model construction are flawed and varied in the ED research field. It is CN crush injury that is the most commonly used method in recent years. This study aims to provide a detailed description of the procedure of bilateral CN injury rat model construction and measurement of intracavernous pressure (ICP) recording, providing a reliable and reproducible CN injury rat model. This work successfully developed the CN injury method of hemostat crush injury using a syringe needle as hard support and a hemostat with a rubber sleeve. Also, this method concludes that a voltage of 1.0 V, frequency of 20 Hz, and pulse-width of 5 ms are the optimized stimulation parameters for ICP recording in a bilateral CN injury rat model.

研究领域: 泌尿学 · 神经科学 · 生理学
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JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY · 2015 ·Vol. 31 ·期 3 ·679-685 · IF 3.466

Magnetic bead-based AuNP labelling combined with inductively coupled plasma mass spectrometry for sensitively and specifically counting cancer cells

WeiJuan Yang,Zhiming Xi,Xiaoxue Zeng,Ling Fang,Wenjing Jiang,Yongning Wu,LiangJun Xu,FengFu Fu

Early diagnostic methods are the most effective way to increase the survival rate of cancer patients. In this study, we present a novel method for sensitively and specifically counting cancer cells using a magnetic bead (MB)-based AuNP–aptamer labelling technique and inductively coupled plasma mass spectrometry (ICP-MS) detection. A MB-based AuNP–aptamer labelling technique can specifically recognize cancer cells and tag AuNPs to the cancer cells, which provides a platform for indirectly counting cancer cells via the detection of Au with ICP-MS. The method reported in this study combines the merits of a MB-based AuNP–aptamer labelling technique and ICP-MS detection, resulting in better specificity and stability, high sensitivity, short analysis time, and robust resistance to a complicated matrix. Especially, the employment of ICP-MS detection and the presence of MBs that facilitate the magnetic separation of target cells, not only greatly shorten the analysis time but also greatly enhance the resistance of our method to a complicated matrix. The proposed method can be used to count as few as 100 human hepatocellular carcinoma SMMC-7721 cells in 1 mL of serum with a recovery of 93–104% and a RSD < 4% (n = 5) within 3 hours. The success of this study provides a promising rapid approach for the early detection of human hepatocellular carcinoma cells in clinical diagnosis.

CAS / MDL: 16961-25-4
研究领域: 分析化学 · 癌症生物学 · 医学诊断
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ANALYTICA CHIMICA ACTA · 2026 · IF 6

A novel and efficient single column separation procedure for high-precision determination of Molybdenum isotope ratio analysis by MC-ICP-MS

Bingyu Peng,Qiaohui Zhong,Feiyu Dong,Gaobin Chu,Lu Yin,Jing Zhang,Jie Li

Background Molybdenum (Mo) isotope has been widely used to trace various redox processes in earth science, however, conventional separation methods, typically depend on toxic hydrofluoric acid (HF), redox reagents (e.g., hydrogen peroxide (H 2 O 2 ) and ascorbic acid (HAsc)), or multi-column purification steps, which introduce either safety hazards or operational complexity. In this study, a safe and efficient single-column procedure without use of either HF or redox reagents was developed for Mo separation from various samples for high precision Mo isotope measurements. Results This method takes advantage of high selective adsorption of Mo on an in-house TOPO resin and only utilize the diluted HCl - HNO 3 media, achieving an effective matrix removal, a high Mo recovery (>93 %) and low procedural blanks (<0.50 ng). Repeated analyses of NIST SRM 3134, Mo metal, and seawater CASS-6 yielded an external reproducibility better than ±0.06 ‰ (2SD). Mn-doping experiments revealed that Mn/Mo ratios exceeding 0.50 induced significant polyatomic interference, causing measurable negative shifts (>0.10 ‰) in δ 98/95 Mo NIST SRM 3134 values. The method was validated using 11 geological reference materials, showing good agreement with published values. Additionally, the δ 98/95 Mo NIST SRM 3134 values of five biological reference materials (e.g., green tea, human hair, pig liver, and fetal bovine serum) were reported for the first time, exhibiting a significant isotopic variation of 1.44 ‰. Significance and novelty Compared with anion/cation-exchange resins or extraction resins, this novel procedure based on in-house TOPO resin depends on dilute HCl - HNO 3 media and effectively purifies Mo from the matrix, with good performance and operational safety. Additionally, the δ 98/95 Mo NIST SRM 3134 values for biological reference materials provide valuable references for quality assurance and inter-laboratory comparisons in emerging applications of Mo isotopes in biological systems. Overall, this study provided a simpler and safer alternative method for high-precise determination of Mo isotope in various samples.

CAS / MDL: 78-50-2
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