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JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY · 2016 ·Vol. 31 ·期 11 ·2285-2292 · IF 3.379

Speciation analysis of silver sulfide nanoparticles in environmental waters by magnetic solid-phase extraction coupled with ICP-MS

Xiaoxia Zhou,Jingfu Liu,Chungang Yuan,Yongsheng Chen

The growing production and widespread application of silver nanoparticles (AgNPs) have led to their release into the environment, where they are mostly transformed to silver sulfide nanoparticles (Ag2S NPs). Thus, speciation analysis of Ag2S NPs in environmental matrices is essential for understanding the environmental process and toxic effects of AgNPs. Herein, we report the use of aged iron oxide magnetic particles (IOMPs) as magnetic solid-phase extraction adsorbents for speciation analysis of Ag2S NPs. It was found that IOMPs are excellent adsorbents for the selective extraction of silver-containing nanoparticles (AgCNPs) including Ag2S NPs, AgNPs and AgCl NPs in the presence of Ag+. More importantly, Ag2S NPs can be distinguished from the other AgCNPs by sequential elution. After pre-eluting AgNPs and AgCl NPs as Ag+ with 2% (v/v) acetic acid and IOMPs as the sacrificial oxidants, Ag2S NPs were completely eluted as a Ag(I) complex by 10 mM thiourea in 2% (v/v) acetic acid and quantified directly by inductively coupled plasma mass spectrometry (ICP-MS). While the extraction of Ag+ was negligible, the maximum extraction of AgCNPs by IOMPs was attained at pH 4.9–6.2, and the interference of humic acid in the AgCNP extraction can be efficiently eliminated by adding Ca2+. Under optimized conditions, the method provides low detection limit (0.068 μg L−1) and high reproducibility (relative standard deviations < 5.1%) for Ag2S NPs. By simultaneously spiking 0.16–10.3 μg L−1 AgNPs and 0.53–14.8 μg L−1 Ag2S NPs, the Ag2S NP recoveries were in the range of 69.6–100.2% for the tap, river and lake waters; and in the range of 106.2–149.9% for the WWTP effluent due to the part sulfidation of AgNPs to Ag2S NPs. Our method is valid for the speciation analysis of Ag2S NPs in water samples, which provides an efficient approach for studying the sulfidation of AgNPs and Ag+.

研究领域: 环境科学 · 分析化学
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JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY · 2024 ·Vol. 39 ·期 5 ·1353-1360 · IF 3.1

Purification of boron using a combination of cationic and boron-specific resins and determination of boron isotopic composition in sediments by MC-ICP-MS

Ning Zhang,Xue-Qin Wen,Mao-Yong He,Tongxiang Ren,Li Deng,Yuanyuan Cheng,Xiaolin Zhang,Junhua Guo

Boron, as both a lithophilic and biophilic element with high solubility, provides profound insights into the history of the Earth and environmental changes through its isotopes present in sediments. However, there are still some challenges in the accurate and precise determination of boron isotopes in sediments, particularly in pre-processing. When using boron-specific resins for the purification and enrichment of boron, it is in an alkaline environment. During the pre-treatment process, insoluble hydroxides of Al, Fe, and rare earth elements precipitate, exhibiting strong boron adsorption in high-pH solutions. This has potential impacts on the accuracy of boron isotope measurements. This study assesses a method that uses Na2CO3 and K2CO3 for dissolution at reduced temperatures and a cationic resin combined with a boron-specific resin for the enrichment and purification of boron in sediments. All the Al, Fe, and rare earth elements, which can generate water-insoluble hydroxides, were mainly removed by the cationic resin column, and boron in the sample solutions without Al, Fe, and rare earth elements was extracted by the boron-specific resin. The boron isotope composition (δ11B) was determined using MC-ICP-MS. The results indicate that this method fully decomposes and efficiently purifies the sediments. The long-term instrumental external reproducibility of δ11B values for NIST SRM 951a, ERM-AE120, and ERM-AE121 were 0.01 ± 0.09‰ (n = 13), −20.28 ± 0.16‰ and 19.98 ± 0.14‰, based on the measurements using a series of international reference materials over the last three years. The measured δ11B values for the standards have various matrices. The δ11B values of GSR-1 (−13.14‰ ± 0.27‰), BHVO-2 (−0.66 ± 0.06‰), AGV-2 (−3.22 ± 0.14‰) and Nass-6 (39.83 ± 0.07‰) are in agreement with the published data within uncertainty. The samples from Sihailongwan Maar Lake (SMK), the Loess Plateau (Loess-1 and Loess-2), shale (SH-1 and SH-2), and basalt (BL-1 and BL-2) were treated. The δ11B values for SMK, Loess-1, and Loess-2 are −10.20 ± 0.29‰, −11.06 ± 0.16‰, and −10.79 ± 0.10‰, showing a close relationship with δ11B of the continental crust. The δ11B values for shale (SH-1 and SH-2) are −7.06‰ ± 0.32‰ and +2.28‰ ± 0.05‰, while those for basalt (BL-1 and BL-2) are −8.78‰ ± 0.09‰ and +2.50‰ ± 0.19‰. These results indicate a significant variation in the δ11B values across these samples. These findings imply that this approach is capable of efficiently enriching and purifying boron in sediments. It enables accurate and precise determination of δ11B in sediments, thus offering a reliable tool for conducting boron isotope studies in sedimentary earth science.

研究领域: 地球化学 · 环境科学 · 分析化学
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MICROCHEMICAL JOURNAL · 2017 · IF 3.034

Visible light photochemical vapor generation using metal-free g-C3N4/CQDs composites as catalyst: Selective and ultrasensitive detection of mercury by ICP-MS

Jingrong Zhou,Yunfei Tian,Xi Wu,Xiandeng Hou

Photochemical vapor generation (PCVG) is a green and effective sampling technology for analytical atomic spectrometry , and in recent years it has been received continuous attention. In this work, visible light photochemical vapor generation was achieved with metal-free g-C 3 N 4 /CQDs (carbon nitride/carbon quantum dots) composites as a photocatalyst, and used for selective and ultrasensitive detection of total mercury by inductively coupled plasma mass spectrometry (ICP-MS). The limit of detection can be as low as 8   ng   L −   1 , making it one of the most sensitive methods for mercury determination . The visible light photochemical vapor generation can also be coupled to other analytical atomic spectrometric techniques.

CAS / MDL: 64-18-6 108-78-1
研究领域: 分析化学 · 环境科学
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SCIENCE OF THE TOTAL ENVIRONMENT · 2021 · IF 7.963

Enzyme digestion combined with SP-ICP-MS analysis to characterize the bioaccumulation of gold nanoparticles by mustard and lettuce plants

Wen-Jing Wei,Lei Li,Yu-Pei Gao,Qiang Wang,Yao-Yu Zhou,Xin Liu,Yuan Yang

Plants can absorb and accumulate engineered nanomaterials (ENMs) through water and soil, providing a potential way for nanoparticles to be enriched in humans through the food chain. In this paper, a combination of enzymatic digestion method and SP-ICP-MS analysis was used to quantitatively characterize the enriched AuNPs in mustard and lettuce plants. The results showed that Macerozyme R-10 enzyme can extract AuNPs from plants without obvious aggregation/dissolution. Both mustard and lettuce plants can absorb and enrich the complete AuNPs to the above-ground organs, and the particle number concentrations detected are 1.24 × 10 7 particles L −1 and 4.39 × 10 7 particles L −1 , respectively. With different exposure level of AuNPs(0.5 mg L −1 ,), a particle number concentration of 2.32 × 10 7 particles L −1 was detected in the stems of lettuce plants, while the mustard failed to transport AuNPs to the above-ground organs. The transport efficiency of Au ions by plants is higher than that of AuNPs, and the plants have stronger bioavailability for ions.

研究领域: 植物学 · 环境科学 · 纳米毒理学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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ECOTOXICOLOGY AND ENVIRONMENTAL SAFETY · 2019 · IF 4.527

Distribution and chemical forms of cadmium in Coptis chinensis Franch. determined by laser ablation ICP-MS, cell fractionation, and sequential extraction

Wenli Huang,Zhenqing Bai,Jie Jiao,Honglin Yuan,Zhian Bao,Shaoning Chen,Meihai Ding,Zongsuo Liang

Coptis chinensis Franch., is a widely used medicinal plant in China. This plant is often contaminated by cadmium (Cd) and render health risk to human consumers. Understanding distribution of Cd and its chemical forms is important to evaluate accumulation of the metal and its detoxification mechanisms in this plant. Since few studies have focused on this aspect, we used laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) to spatially locate Cd in rhizome cross-sections, and ICP-MS to analyze the Cd subcellular distribution and the chemical forms of Cd in different tissues. Rhizome bioimaging results showed that Cd was distributed predominantly within the periderm, cortex, pith, and root trace vascular bundle. The LA-ICP-MS results suggested that Ca 2+ channels might be a pathway for Cd entry into the plant. Subcellular distribution data indicated that most of Cd was associated with the cell wall (41.8–77.1%) and the soluble fraction (14.4–52.7%) in all tissues. Analysis of chemical forms revealed that majority Cd existed in less mobile and less toxic forms in all tissues, and P could convert to insoluble phosphate with Cd to moderate Cd toxicity. The new understanding of Cd accumulation and detoxification might provide novel strategies for reducing the levels of Cd in C. chinensis Franch., thereby mitigating its potential transfer to humans and providing a theoretical basis for evaluating the Cd status in other medicinal plants. Further, our findings might provide a basis for establishing a reasonable Cd limit level of traditional Chinese medicinal materials.

研究领域: 植物学 · 环境科学 · 药用植物研究
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ENVIRONMENTAL SCIENCE & TECHNOLOGY · 2023 · IF 11.4

Determination of the Particle Number Concentration, Size Distribution, and Species of Dominant Silver-Containing Nanoparticles in Soils by Single-Particle ICP-MS

Qingsheng Bai,Qingcun Li,Jingfu Liu

The potential risk of various silver-containing nanoparticles (AgCNPs) in soils is related to the concentration, size, and speciation, but their determination remains a great challenge. Herein, we developed an effective method for determining the particle number, size, and species of dominant AgCNPs in soils, including nanoparticles of silver (Ag NPs), silver chloride (AgCl NPs), and silver sulfide (Ag2S NPs). By ultrasonication wand-assisted tetrasodium pyrophosphate extraction, these AgCNPs were extracted efficiently from soils. Then, multistep selective dissolution of Ag NPs, AgCl NPs, and whole Ag NPs/AgCl NPs/Ag2S NPs was achieved by 1% (v/v) H2O2, 5% (v/v) NH3·H2O, and 10 mM thiourea in 2% (v/v) acetic acid, respectively. Finally, the particle number concentration and size distribution of AgCNPs in the extracts and the remaining AgCNP particle number concentration after each dissolution were determined by single-particle inductively coupled plasma mass spectroscopy for speciation of the dominant AgCNPs. AgCNPs were detected in all five soil samples with the concentrations of 0.23–8.00 × 107 particles/g and sizes of 16–110 nm. Ag2S NPs were the main form of AgCNPs in the examined soils with the percentage range of 53.98–69.19%, followed by AgCl NPs (11.42–23.31%) and Ag NPs (7.78–16.19%). Our method offers a new approach for evaluating the occurrence and potential risk of AgCNPs in environmental soils.

CAS / MDL: 25249-54-1 9003-39-8
研究领域: 环境科学 · 分析化学
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ANALYTICA CHIMICA ACTA · 2023 · IF 6.2

Ultrasensitive determination of selenium in water and food samples by ICP-MS: UiO-66-NH2 for preconcentration and direct slurry hydride generation

Qing Yang,Chenghui Li,Jing Hu,Xiandeng Hou

Background Selenium is an indispensable microelement for humans and food is the main source of selenium intake. As one of the best techniques for the determination of selenium, inductive coupling plasma-mass spectrometry (ICP-MS) features some unique advantages, such as wide linear range and high sensitivity. Nevertheless, it still remains a challenge to achieve the accurate and high sensitivity determination of ultra-trace selenium in food samples by ICP-MS owning to the high first ionization energy of selenium and interferences from sample matrices as well as isobaric interferences. Results In this work, UiO-66-NH 2 (metal organic framework, MOF) was fast synthesized by microwave method and employed for the preconcentration of ultra-trace selenium with an adsorption efficiency of nearly 100 %. The selenium-adsorbed MOF was collected by filtration, and then simply converted to slurry for in situ hydride generation (HG) for sensitive detection of selenium by ICP-MS. Various factors affecting the adsorption of selenium by the MOF (including pH, adsorption time, and amount of MOF) together with main parameters of hydride generation (including concentrations of HCl and NaBH 4 ) were carefully evaluated. Experimental results show that effective matrix separation can greatly reduce interference, with an excellent detection limit of 1 ng/L. The practicability and accuracy of this method were successfully confirmed by the determination of trace selenium in several food samples. Significance UiO-66-NH 2 (MOF) was used as an effective adsorbent for the preconcentration of selenium prior to direct slurry sampling HG-ICP-MS determination. Direct slurry sampling avoided additional elution procedures and was conducive to eliminating matrix and isobaric interferences. High sensitivity and interference-free determination were achieved for determination of ultra-trace Se in complex food samples.

CAS / MDL: 10312-55-7
研究领域: 分析化学 · 环境科学 · 食品安全
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ANALYTICA CHIMICA ACTA · 2020 · IF 5.977

Determination of trace elements in high-purity quartz samples by ICP-OES and ICP-MS: A normal-pressure digestion pretreatment method for eliminating unfavorable substrate Si

Xuelin Dong,Yuxiang Xiong,Nan Wang,Zhou Song,Jie Yang,Xiumei Qiu,Lihua Zhu

The analysis of siliceous matrix samples may adopt a two-step pretreatment , which includes melting with ammonium hydrogen fluoride and redissolving with nitric acid . However, the residual of substrate silicon unfavorable to the determination of trace elements in the samples due to serious matrix effects. Here, a new digestion method using simultaneously both ammonium bifluoride and nitric acid under normal pressure was developed for high-purity quartz sand sample. The digestion pretreatment is a two step process: melting/dissolving with both ammonium bifluoride and nitric acid at 200 °C for 2 h, and evaporating the solution at 250 °C to dryness. As confirmed by XRD analysis, silicates in the sample were converted to (NH 4 ) 3 SiF 6 NO 3 in the melting/dissolving step. TGA analysis shows that the generated (NH 4 ) 3 SiF 6 NO 3 could be decomposed and evaporated completely at 250 °C, which ensured a complete removal of silicon by the followed evaporation of the solution at 250 °C. As a result, the followed ICP-OES and ICP-MS analysis needed a solution dilution of only 100 times for the determination of Ca, Mg, Al, Rb, Ba, REE and other trace elements. The new method was applied to the analysis of three certified reference materials, and the results were well consistent with the standard value with RSD% values between 0.62% and 9.73%. Therefore, this method can be applied to the analysis of trace elements in high purity silica-based samples, with the advantages of time-saving, small dilution factor (only 100 times) and low detection limit.

研究领域: 分析化学 · 材料科学
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JOURNAL OF RADIOANALYTICAL AND NUCLEAR CHEMISTRY · 2025 · IF 1.6

A rapid method for determination of ultra-trace level Pu isotopes in atmospheric particulate matter samples using SF-ICP-MS and TEVA resin

Xin Futao,Luo Min,Li Chun,Ma Lingling,Xu Diandou,Xu Gang,Li Xi,Shao Yang

A rapid method has been developed for determining ultra-low level Pu isotopes in atmospheric particulate matter samples using SF-ICP-MS and TEVA resin. The Pu purification, ashing conditions and microwave digestion, were optimized to achieve high decontamination factor of U (4.1 × 10 4 ) and stably high Pu recovery (80–90%). The method detection limits were estimated to be 0.83 fg/g for 239 Pu and 0.70 fg/g for 240 Pu. Four IAEA certified reference materials were used for method evaluation. Finally, the method was successfully applied to determine the source of Pu in atmospheric particulate matter samples. The method can be performed within 16 h.

研究领域: 环境科学 · 核化学 · 分析化学
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NEW JOURNAL OF CHEMISTRY · 2019 ·Vol. 43 ·期 9 ·3946-3955 · IF 3.069

Single particle ICP-MS and GC-MS provide a new insight into the formation mechanisms during the green synthesis of AgNPs

Huiling Zhang,Yuxiong Huang,Jianqiang Gu,Arturo Keller,Yuwei Qin,Yue Bian,Kun Tang,Xiaolei Qu,Rong Ji,Lijuan Zhao

Green synthesis of metallic nanoparticles (NPs) using plant extracts has received considerable attention due to its environmentally and economically friendly nature. Various metabolites in plants such as amino acids, organic acids, sugars and phenolic compounds have been speculated to be responsible for the synthesis of metallic NPs in previous studies. However, to date, there has been a lack of direct evidence linking specific metabolites to the reduction of metal ions to form metallic NPs. Here, AgNPs are synthesized using cucumber leaf extract and characterized by UV-visible spectroscopy, dynamic light scattering (DLS) and transmission electron spectroscopy (TEM). Single particle inductively coupled plasma mass spectrometry (sp-ICP-MS) was used to investigate the size of newly synthesized NPs as well as the kinetics of particle formation. Gas chromatography–mass spectrometry (GC-MS) based metabolomics identified and quantified 245 metabolites in cucumber leaf extracts. By comparing the concentrations of metabolites before and after the reaction, the metabolites responsible for the synthesis were screened out. Reducing sugars (cellobiose, ribulose-5-phosphate, melibiose, 2-deoxy-D-glucose, tagatose, fructose, ribose, 3,6-anhydro-D-galactose) were markedly decreased after the reaction, indicating that reducing sugars are involved in the biosynthesis process and possibly function as reducing agents. The key thermodynamic data of the reaction between Ag+ and reducing sugars were obtained by using isothermal titration calorimetry (ITC), which further confirmed the interaction between Ag+ and metabolites. This study provides a deep insight into the reaction process and mechanism of green synthesized AgNPs.

CAS / MDL: 1336-21-6
研究领域: 环境科学 · 纳米生物学
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ANALYTICA CHIMICA ACTA · 2025 · IF 6

LA-ICP-MS-quantitated boronate affinity magnetic Zr-MOFs prepared via post-modification for glycopeptides enrichment

Feng Zhang,Sen Zhang,Xing Liu,Wei Gao,Jun Luo,Yi-fan Pan,Wei-Juan Zheng,Xin Hu,Hong-zhen Lian

Background Glycoproteins are critical in various biological processes and attract lots of attention of researchers. It still remains a challenge to detect glycopeptides by mass spectrometry because of their low abundance with heterogeneity and lability, as well as signal suppression by non-glycopeptides. The boronate affinity-based enrichment is an effective solution for detecting cis -diols-containing compounds including glycopeptides in complex matrices. However, there has not been any report about absolute quantitation of boron in the absorbent materials for glycopeptides, which obstructed the tailored design of boronate affinity materials and deeper understanding of interaction mechanisms. Results This work presents the development of a boronic acid-functionalized magnetic zirconium metal-organic framework (mMOF–AAPBA) with actual boron content for specific capture of glycopeptides. The synthesized nanocomposite could enrich glycopeptides by magnetic solid-phase extraction (MSPE) via the synergistic effect of hydrophilic interaction and boronate affinity. After full characterization including quantitative analysis of boron by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), mMOF–AAPBA was applied as MSPE absorbent to capture glycopeptides. Under the optimized conditions, it could enrich 28 glycopeptides both from horseradish peroxidase and immunoglobulin digests, with a limit of detection of 1 fmol μL −1 coupled with matrix-assisted laser desorption/ionization time of flight mass spectrometry. The boronate affinity absorbent also possessed great ability of anti-interference and good reusability. Furthermore, it possessed high performance in enriching glycopeptides in real samples including human saliva and traditional Chinese medicine injections. Significance In the preparation of the boron-containing nanocomposites, there is a special interest that an accurate protocol was established to assay boron based on LA-ICP-MS assisted by home-made matrix reference substances for the first time. These findings highlight the quantitative boron-containing mMOF–AAPBA as a robust affinity material for glycopeptide enrichment in real biological samples, offering potential applications in glycoproteomics and other cis -diols compound related researches.

研究领域: 分析化学 · 生物化学 · 纳米技术 · 质谱学 · 糖蛋白质组学
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CHROMATOGRAPHIA · 2018 ·Vol. 81 ·期 6 ·881-889 · IF 1.401

Determination of Metallothionein Isoforms in Fish by Cadmium Saturation Combined with Anion Exchange HPLC-ICP-MS

Li Shan,Yang Zhaoguang,Cao Junfei,Qiu Bo,Li Haipu

Abstract The content of metallothionein (MT) in fish can serve as a biomarker for heavy metal contamination in an aquatic environment. In this paper, an improved sample separation and quantification method using cadmium saturation combined with anion exchange high performance liquid chromatography–inductively coupled plasma mass spectrometry (HPLC–ICP-MS) was developed to measure the two major isoforms of MT (MT-I and MT-II) in fish. Replacing sulfur with cadmium as the quantitative element by cadmium saturation reduced the instrumental requirement and analysis cost. In the chromatographic separation, NH 3 –NH 4 Cl buffer was applied as the mobile phase instead of Tris–HCl buffer to prevent carbon deposition on the ICP cone. The chloride concentration was found to be a key factor to the separation of MT-I and MT-II, and the optimum chromatographic condition was 27 mM of NH 3 –NH 4 Cl in isocratic mode, with a pH of 8.6 and a flow rate of 0.8 mL min −1 . The limits of detection were 0.7 μg g −1 for MT-I and 1.0 μg g −1 for MT-II, with recoveries ranging from 96.2 to 104.2% for MT-I and 84.7 to 90.4% for MT-II in different fish tissues. The relative standard deviations were less than 8% for both isoforms. Graphical abstract

研究领域: 环境科学 · 分析化学 · 毒理学
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