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MOLECULES · 2022 ·Vol. 27 ·期 9 ·2982 · IF 4.927

Multi-Element Analysis and Origin Discrimination of Panax notoginseng Based on Inductively Coupled Plasma Tandem Mass Spectrometry (ICP-MS/MS)

Chao Ji,Jinyu Liu,Qin Zhang,Juan Li,Zhiqiang Wu,Xingyu Wang,Yuxin Xie,Jiangchao Zhao,Rui Shi,Xing Ma,Mohammad Rizwan Khan,Rosa Busquets,Xiahong He,Youyong Zhu,Shusheng Zhu,Wenjie Zheng

Panax notoginsengis an important functional health product, and has been used worldwide because of a wide range of pharmacological activities, of which the taproot is the main edible or medicinal part. However, the technologies for origin discrimination still need to be further studied. In this study, an ICP-MS/MS method for the accurate determination of 49 elements was established, whereby the instrumental detection limits (LODs) were between 0.0003 and 7.716 mg/kg, whereas the quantification limits (LOQs) were between 0.0011 and 25.7202 mg/kg, recovery of the method was in the range of 85.82% to 104.98%, and the relative standard deviations (RSDs) were lower than 10%. Based on the content of multi-element inP. notoginseng(total of 89 mixed samples), the discriminant models of origins and cultivation models were accurately determined by the neural networks (prediction accuracy was 0.9259 and area under ROC curve was 0.9750) and the support vector machine algorithm (both 1.0000), respectively. The discriminant models established in this study could be used to support transparency and traceability of supply chains ofP. notoginsengand thus avoid the fraud of geographic identification.Keywords:Panax notoginseng;ICP-MS/MS;multi-element;origin discrimination;cultivation model discrimination

CAS / MDL: 7664-39-3
研究领域: 植物学 · 药学 · 分析化学
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APPLIED MICROBIOLOGY AND BIOTECHNOLOGY · 2019 ·Vol. 103 ·期 3 ·1475-1483 · IF 3.67

Quantitative determination of trace metals in single yeast cells by time-resolved ICP-MS using dissolved standards for calibration

Liu Zihui,Xue Aifang,Chen Hao,Li Shengqing

Time-resolved inductively coupled plasma mass spectrometry (ICP-MS) for studying cellular heterogeneity or detecting metals in single cells draws increasing attention in the recent years. Considering the full width of a single-cell event is about 0.5–0.9 ms, dependent on the duration of the ion plume generation in typical ICP condition, dwell time shorter than the transient event was suggested for fully profiling it. Herein we investigated the effect of dwell time (0.1–10.0 ms) on the signal profiles of single-cell events, signal-to-background ratio, duty cycle of detection, the limit of detection, and the ability of cell counting by the time-resolved ICP-MS, using yeast ( Saccharomyces cerevisiae ) cells as example. Two calibration equations with respect to the length of dwell time (0.1 ms or 5.0 ms), simply using dissolved metal standard solutions, were constructed and successfully applied to the determination of K, Mg, Zn, Mn, and Cu in single yeast cells. The limit of detection (LOD, fg per cell) obtained at dwell time 0.1 ms was 1.68 (K), 0.29 (Mg), 0.17 (Zn), 0.01 (Mn), and 0.02 (Cu) for single-cell analysis of yeast cells; the LOD (fg per cell) at 5.0 ms was 80.0 (K), 10.3 (Mg), 1.6 (Zn), 0. 14 (Mn), and 0.24 (Cu), respectively. The results showed that a short dwell time leading to high signal-to-background ratio and low LOD was a prerequisite for the quantitative analysis of ultra-trace content of metals in single cells.

研究领域: 分析化学 · 生物化学
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TALANTA · 2018 · IF 4.244

Polymer monolithic capillary microextraction on-line coupled with ICP-MS for determination of inorganic selenium species in natural waters

Chao Wang,Man He,Beibei Chen,Bin Hu

In this work, ethylenediamine modified poly(glycidyl methacrylate-ethylene dimethacrylate)(poly(GMA-EDMA-NH 2 )) was prepared for highly selective extraction of Se(VI) with high adsorption capacity of 0.825 mg m −1 (530 µm i.d.). Based on it, a novel method of polymer monolithic capillary microextraction (CME) on-line coupling with inductively coupled plasma-mass spectrometry (ICP-MS) was developed for the determination of inorganic selenium species (Se(IV)/Se(VI)) in natural waters. Under the optimized conditions, the analytical performance of the proposed on-line CME-ICP-MS method was evaluated for Se(VI). The limit of detection for Se(VI) was 14.2 ng L −1 , and the enrichment factor was 50-fold with the sample throughput of 5 h −1 . For Se(IV), the concentration was obtained by subtracting Se(VI) from the total Se(VI) obtained by the proposed method after oxidation of Se(IV) to Se(VI). The accuracy of the method was validated by the analysis of a Certified Reference Materials of GBW(E)080395. The proposed method was applied for the analysis of inorganic selenium species in natural waters with good recoveries. The developed method of monolithic CME-ICP-MS is sensitive, simple and rapid for the analysis of inorganic selenium species in natural waters.

研究领域: 分析化学 · 环境科学
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JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY · 2022 ·Vol. 38 ·期 2 ·449-456 · IF 4.351

An efficient method for the separation of REEs from Ba for the accurate determination of REE content in Ba-rich samples by ICP-MS

Wengang Liu,Yuchen An,Qinyuan Qu,Pengfei Li,Lixin Zhang,Chaofeng Li,Shuang Wei,Hongying Zhou,Jiubin Chen

Barium (Ba) is a major element in many geological samples (e.g. barite/witherite-rich samples) and introduces serious oxide and hydroxide interferences during the analysis of rare earth elements (REEs) by ICP-MS. Hence, eliminating Ba interference is an indispensable step for accurate ICP-MS analysis of REEs. Though ion-exchange chromatography is widely used for REE purification, the tediousness, time consumption and high cost limit the application of this purification method. In this study, we developed a rapid and reliable separation method to eliminate Ba from geological samples for the precise measurement of REEs by ICP-MS. The new method was established based on the difference in solubility between Ba and REEs in concentrated nitric acid as barium nitrate (Ba(NO3)2) is almost insoluble, in contrast to REEs. The whole separation procedure could be completed in less than two hours and only consumed 1.5 mL 15 M nitric acid. The protocol resulted in acceptable procedural blanks (below 0.02 ng mL−1), quantitative recovery (96–103%) of REEs, and limited Ba content (0.37 ± 0.14 μg mL−1, (2SD, n = 50)) in the purified solution (50 mL), in which the interference effect could be eventually eliminated by mathematical correction during the ICP-MS analysis. The method was successfully applied to four natural barite-rich samples with BaSO4 content ranging from 18.87 wt% to 42.41 wt%. Overall, this accurate and rapid method shows great potential for the precise determination of the REE content in Ba-rich samples by ICP-MS.

CAS / MDL: 10361-37-2
研究领域: 分析化学 · 地球化学
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JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY · 2022 ·Vol. 38 ·期 1 ·156-165 · IF 4.351

Accurate determination of rare earth elements in small volumes of porewater from marine sediments by laser ablation solution sampling ICP-MS

Xiuhong Liao,Wen Zhang,Tao Yang,Zhaochu Hu,Tao Luo,Xianli Zeng,Lian Zhou

Rare earth elements (REEs) in porewater can be useful proxies in the studies of marine geochemistry. The main challenges for the determination of REEs in porewater samples from marine sediments lie in three aspects—low concentration, high salinity, and limited sample sizes (usually only a few millilitres). In this study, a method based on laser ablation (LA) solution sampling ICP-MS for REEs analysis of small volumes (2–4 mL) of porewater is established. With the help of matrix removal and REEs preconcentration from natural liquids by a miniaturized Fe(OH)3 co-precipitation method, a high enrichment factor (10–20 fold) was achieved with only 2 mL of the original liquid, which was preconcentrated to be as small as 100–200 μL. Ultratrace (sub-pg mL−1) analysis was realized through the use of high laser ablation pulse frequency (up to 250 Hz) and based on the high transport efficiency of aerosol particles by the LA system. Due to the almost “dry” ICP condition generated by LA and nitrogen addition (5 mL min−1) to the plasma, the CeO+/Ce+ ratio was reduced to approximately 0.05%, and the total yields of BaO+ and BaOH+ ions were reduced to 0.003%, which means that the potential biases induced by oxide and hydroxide interferences could be negligible. Method validation was achieved through the analysis of the seawater reference material NASS-7 and a spike recovery test with quantitative recoveries of 94–101% for REEs. The application results of porewater samples characterized by no or slight Ce anomalies together with significantly positive Eu anomalies may be indicative of highly reducing and neutral to basic pH conditions. Reagents consumed by the LA-ICP-MS method were significantly reduced, making it a more environment-friendly method. Moreover, the simplicity in sample preparation and lack of need for special reagents or devices give the proposed method great potential for wide applications in the determination of REEs in natural water samples.

CAS / MDL: 1336-21-6
研究领域: 海洋化学 · 分析化学
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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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ANALYTICAL LETTERS · 2025 · IF 1.8

Determination of Platinum Group Metals in Catalysts by Inductively Coupled Plasma–Atomic Emission Spectrometry (ICP-AES) with Coprecipitation Separation and Enrichment

Feng Yang,Yonghai Yuan,Jiacai Li,Yihua Shi

This study presents a method for determining platinum group metals (Pt, Pd, and Rh, PGMs for short) in metallic catalysts using inductively coupled plasma–atomic emission spectrometry (ICP-AES) with coprecipitation separation and enrichment. The monolithic catalysts were initially digested using ultrasonic-assisted HCl dissolution followed by Na2O2 melting and filtration of the residue, overcoming the challenge of uniform grinding catalyst samples. Subsequently, coprecipitation with polyethylene oxide (PEO) and Te was employed to mitigate interferences from Si and other elements. ICP-AES was then used for the determination of PGMs. In this method, co-existing elements, such as 200 mg·L−1 of Te and 10 mg·L−1 of Fe, Cr, Ni, Al, and Na, exhibit no interference in the quantification of PGMs. The limits of detection (3s) were 0.04, 0.016, and 0.014 μg·g−1 for Pt, Pd, and Rh, respectively. The limits of quantification (10s) were 0.13, 0.053, and 0.046 μg·g−1 for Pt, Pd, and Rh, respectively. The relative standard deviations (RSD, n = 7) ranged from 1.36% to 2.61% for Pt, 1.14% to 3.25% for Pd, and 1.89% to 3.78% for Rh, indicating the method’s robustness and precision. Comparative analysis of the results obtained from six metallic catalyst products using this method and flame atomic absorption spectrometry (FAAS) reveals consistent results, further confirming the proposed method’s reliability and feasibility for determining PGMs in metallic substrate catalysts.

CAS / MDL: 68441-17-8
研究领域: 分析化学 · 环境科学 · 材料科学
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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
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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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