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MICROCHEMICAL JOURNAL · 2020 · IF 3.594

Hybrid monolith assisted magnetic ion-imprinted polymer extraction coupled with ICP-MS for determination of trace Au(III) in environmental and mineral samples

Yu Hua,Jia-yuan Li,Hong Min,Xiao-hong Wu,Xiao-bing Cui,Yi-jun Chen,Hong-zhen Lian,Dong Sheng

In this work, by introducing solvothermal method for generating Fe 3 O 4 nanoparticles and “one-pot” method for synthesizing organic–inorganic hybrid monolithic vinyl functionalized Fe 3 O 4 (Fe 3 O 4 @HM), a facile procedure was proposed for preparing poly(1-vinylimidazole) (PVIM) functionalized gold ion imprinted polymer based MNPs@IIP (MNPs@HM@PVIM-Au-IIP). The as-prepared magnetic nanocomposites were characterized by scanning electron microscopy (SEM), transmission electron microscope (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), and vibrating sample magnetometry (VSM), etc. After the optimum conditions, including solution pH, adsorption time and sample volume, eluent composition and volume, and elution time were investigated, this MNPs@IIP was employed as ion imprinted polymer magnetic solid phase extraction (II-MSPE) matrix for separation and enrichment of trace gold ions followed by inductively coupled plasma mass spectrometric (ICP-MS) determination with excellent selectivity and sensitivity, and strong anti-interference ability. These merits were benefited from the formation of hybrid monolithic interlayer enduing the resultant MNPs@HM@PVIM-Au-IIP with good chemical and mechanical stability, as well as the dimensional homogeneity due to the solvothermal-generated Fe 3 O 4 nanoparticles as the cores. The applicability superiority of this MNPs@IIP was confirmed by the rapid and efficient extraction of trace level Au(III) in environment water, sediment, soil, coal and ore samples with satisfactory results. The reliability of this II-MSPE-ICP-MS method was also verified by using corresponding Certified Standard Reference materials and spiking recovery of the real samples analyzed.

研究领域: 分析化学 · 环境科学 · 材料科学
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TALANTA · 2023 · IF 6.1

Determination of concentrations of Sr and Ba in coal and coal combustion by-products: A comparison between results by ICP-MS and XRF techniques

Xiao Tian,Lei Zhao

Concentrations of trace elements in coal and coal combustion products are commonly analyzed by inductively coupled plasma-mass spectrometry (ICP-MS) due to large number of elements detected and the relatively the low detection limits of this technique. Like other geological samples, complete dissolution of coal and coal combustion products is also essential for accurate ICP-MS results. In this study, Sr and Ba in coal and coal combustion products (fly and bottom ashes) from two coal-combustion power plants from North China analyzed by XRF and ICP-MS were comparatively studied. The concentrations of Sr and Ba analyzed by ICP-MS, when a mixture of acids (2 ml HF + 5 ml HNO 3 for each 50 mg coal sample and 5 ml HF + 2 ml HNO 3 for each 50 mg ash sample) was used for microwave-assisted digestion, do not fit well with the their relative XRF results. This is most probably due to the formation of the fluorides during microwave digestion, and this assumption is supported by the presence of various fluoride compounds, NaMgAl(F, OH) 6 ·H 2 O, NH 4 MgAlF 6 , AlF 3 , and K 2 SiF 6 , in the residues of all the coal and ash samples in our sequential extraction experiment. Cations of Sr and Ba were probably trapped into the divalent cation sites of the fluorides. Concentrations of Sr and Ba analyzed by ICP-MS using increased HF and HF/HNO 3 ratio (7 ml HF and 2 ml HNO 3 for each 50 mg coal/ash sample) are in better agreement with the XRF results. Our results indicate that excess amount of HF probably has led to the suppression of these elements due to fluoride precipitation. The results indicate that the modified digestion method is capable of achieving complete digestion of coal samples and results in a reliable analysis of Sr and Ba concentrations in coal samples and most fly ashes by ICP-MS. However, the formation of insoluble fluorides is probably not completely suppressed for some bottom ash samples, which can result in underestimation of Sr and Ba concentrations. Nevertheless, XRF analysis can serve as a reliable cross-check method to assist in the evaluation of the accuracy of ICP-MS results.

CAS / MDL: 7697-37-2
研究领域: 环境科学 · 分析化学 · 地球化学
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MICROCHEMICAL JOURNAL · 2024 · IF 4.9

Label-free and sensitive assay for ICP-MS determination of alkaline phosphatase activity via manganese target

Yujing He,Jing Hu,Siqi Wei,Chenghui Li,Xiandeng Hou

As an essential and universal enzyme, alkaline phosphatase (ALP) has been identified as an important biomarker of various diseases, thus highly sensitive assay of ALP activity is of great significance. Herein, a label-free and sensitive ICP-MS based assay was developed for ALP activity detection using MnO 2 nanosheets (MnO 2 NS) as the element target source. ALP triggered the hydrolysis of ascorbic acid-2-phosphate (AAP) to produce reductive ascorbic acid (AA), followed with the decomposition of MnO 2 NS to Mn 2+ ions, which were quantified directly by ICP-MS after selective separation of MnO 2 NS and Mn 2+ ions simply by filtration, and no further elemental labelling was needed. Under the selected conditions, the limit of detection (LOD) was 0.007 U L -1 for ALP. Additionally, this assay was also extended to investigate the inhibition effect of ALP inhibitor (Na 3 VO 4 ) with reasonable results. To our knowledge, this is the first endeavor for ALP activity detection using ICP-MS, which holds great promise for the early clinical diagnosis and biomedical research on ALP.

研究领域: 分析化学 · 生物化学 · 纳米技术 · 医学诊断
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GEOSTANDARDS AND GEOANALYTICAL RESEARCH · 2025 · IF 3.4

A Simple Procedure for Separating Tungsten from Silicate Rocks Prior to Tungsten Isotope Ratio Determination by MC-ICP-MS

Ai-qun Xiao,Pei-pei Zhao,Lu Yin,Bei Xu

A single-column extraction chromatographic purification method for tungsten using the N-benzoyl-N-phenylhydroxylamine (BPHA) resin was investigated in this study. This method greatly simplifies the W purification procedure, and only 10 ml of acid (5 ml 3 mol l -1 HCl-0.1 mol l -1 HF and 5 ml 1 mol l -1 HF) is required to separate W from Ti, Zr, Hf, Ta and other matrix elements. The blank in the separation step was less than 0.1 ng, and the recovery of W was ~ 99%. Six independent digestion measurements of reference materials BHVO-2, BCR-2, RGM-2 and JB-2 yielded μ 182 W values (mean value with intermediate precision, 95% confidence level) of -10.3 ± 4.0 ( n = 6, 2 s ),-1.2 ± 5.3 ( n = 6, 2 s ),-1.4 ± 4.4 ( n = 6, 2 s ) and 0.6 ± 3.8 ( n = 6, 2 s ), respectively, which are in good agreement with the previously reported values.

CAS / MDL: 304-88-1
研究领域: 地球化学 · 分析化学 · 同位素地质学 · 质谱分析
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TALANTA · 2016 · IF 4.035

Speciation analysis of Mn(II)/Mn(VII) using Fe3O4@ionic liquids-β-cyclodextrin polymer magnetic solid phase extraction coupled with ICP-OES

Songqing Chen,Xingxiu Qin,Weixi Gu,Xiashi Zhu

Ionic liquids-β-cyclodextrin polymer (ILs-β-CDCP) was attached on Fe 3 O 4 nanoparticles to prepare magnetic solid phase extraction agent (Fe 3 O 4 @ILs-β-CDCP). The properties and morphology of Fe 3 O 4 @ILs-β-CDCP were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction(XRD), size distribution and magnetic analysis. A new method of magnetic solid phase extraction (MSPE) coupled to ICP-OES for the speciation of Mn(II)/Mn(VII) in water samples was established. The results showed that Mn(VII) and total manganese [Mn(II)+Mn(VII)] were quantitatively extracted after adjusting aqueous sample solution to pH 6.0 and 10.0, respectively. Mn(II) was calculated by subtraction of Mn(VII) from total manganese. Fe 3 O 4 @ILs-β-CDCP showed a higher adsorption capacity toward Mn(II) and Mn(VII). Several factors, such as the pH value, extraction temperature and sample volume, were optimized to achieve the best extraction efficiency. Moreover, the adsorption ability of Fe 3 O 4 @ILs-β-CDCP would not be significantly lower after reusing of 10 times. The accuracy of the developed method was confirmed by analyzing certified reference materials (GSB 07-1189-2000), and by spiking spring water, city water and lake water samples.

CAS / MDL: 822-06-0
研究领域: 分析化学 · 环境科学
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ANALYTICAL LETTERS · 2020 · IF 1.467

Determination of Prussian Blue Nanoparticles in Rat Tissue in the Presence of Endogenous Iron Interferences by Inductively Coupled Plasma – Optical Emission Spectrometry (ICP-OES)

Weimin Ding,Xing Jin,Boyu Ma,Xiaobing Wang,Chenmei Lou,Jian Zheng,Zhiwei Hu,Lijia Jing,Yang Wang

A modified calibration curve method based on the combination of standard addition and traditional calibration curve methods was employed for the quantification of Prussian blue nanoparticles in rats in the presence of endogenous iron interferences. The assay was performed using inductively coupled plasma – optical emission spectrometry (ICP-OES) with yttrium as the internal standard, and validated in biomatrices including liver, heart, kidneys, lungs, spleen and whole blood. For the liver tissue, the intra-day and inter-day precision were 7.84% or less, and the accuracy was between 99.88% and 102.37%. For kidneys, lungs, heart, spleen, and blood, at each exo-additive level from 0.4 to 3.2 µg/mL, the intra-day accuracy was between 98.74% and 102.09%, and the intra-day precision was 6.17% or less. For the addition of no analyte, the intra-day accuracy was between 96.42% and 107.52%, and the intra-day precision was 15.67% or less. The stability was investigated at 25 °C for 24 h and 4 °C for 15 days in liver standard addition samples, and no significant degradation occurred under these conditions. This method was successfully applied to the preliminary pharmacokinetics and tissue distribution study of Prussian blue nanoparticles in rats. This approach may also be applied to the quantification of other ferruginous materials in the biological matrices with endogenous iron.

CAS / MDL: 7697-37-2
研究领域: 分析化学 · 药代动力学 · 生物医学
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MICROCHEMICAL JOURNAL · 2025 · IF 5.1

Multifunctional “four-in-one” effervescent tablet-assisted one step microextraction combined with ICP-OES for determination of lead in Pinellia ternata (Thunb.) Breit

Yan Zhou,Xiaofang Yang,Leshou Zhang,Shaodui Ye,Ya Liu,Ning Lu,Yong Liu,Xiaodong Wen

Developing a fast, simple, and efficient sample pretreatment method is of great practical significance for the analysis of complex matrix samples. In this study, a novel multifunctional “four-in-one” effervescent tablet based on switchable hydrophobic deep eutectic solvent (SHDES) was prepared, which can simultaneously facilitate the in situ synthesis of SHDES and CO 2 generation, phase transition, and phase separation. The effervescent tablet based on the SHDES-assisted microextraction (ETA-SHDES-ME) technique was combined with inductively coupled plasma optical emission spectrometry (ICP-OES) for the determination of Pb 2+ in Pinellia ternata (Thunb.) Breit. The important parameters affecting the extraction efficiency of Pb 2+ were optimized using the Box-Behnken design (BBD). The enrichment factor (EF) and limit of detection (LOD) of the established method for Pb 2+ are 31 and 0.2 μg/L, respectively, offering a fast, simple, and eco-friendly approach, and has the application potential of field analysis.

CAS / MDL: 10051-45-3 141-82-2
研究领域: 分析化学 · 环境科学
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Analytical Methods · 2017 ·Vol. 9 ·期 17 ·2546-2552 · IF 1.9

Simultaneous detection of three gynecological tumor biomarkers in clinical serum samples using an ICP-MS-based magnetic immunoassay

Weizhe Hong,Gongwei Sun,Yi Zhang,Zhi Xing,Biao Huang,Sichun Zhang,Xinrong Zhang

ICP-MS-based multiplex immunoassays have the advantages of low sample consumption and minimized repetitions of tedious procedures. However, this technique is seldom used in clinical tests because of the complicated matrix effect in clinical samples and the discrimination effect to the target proteins. In this work, we developed an ICP-MS-based magnetic immunoassay by using magnetic beads as highly efficient affinity probes and optimizing the magnetic immunoassay parameters. We applied this method to the simultaneous determination of three crucial gynecological tumor biomarkers that are vital in the prognosis and monitoring of the recurrence of breast cancer and ovarian cancer. The measurable ranges of HER-2, HE4 and CA15-3 were 12–1000 ng mL−1, 8–2000 pmol L−1 and 5–200 U mL−1, with detection limits (3σ) of 3.94 ng mL−1, 2.59 pmol L−1 and 1.62 U mL−1, respectively. The relative standard deviations (RSDs) were 2.61% for HER-2 at 15 ng mL−1, 4.90% for HE4 at 25 pmol L−1 and 6.68% for CA15-3 at 10 U mL−1, indicating good accuracy of the method. The spiking test indicated that the present method had a low matrix effect. Under optimized conditions, the simultaneous detection of HER-2, HE4, and CA15-3 in clinical serum samples was performed and the values correlated well with those obtained by the time resolved fluorescence immunoassay (r2 = 0.9568 for HER-2, 0.9485 for HE4, 0.9133 for CA15-3). The present work shows that the ICP-MS-based magnetic immunoassay meets the requirements for the quantification of three crucial gynecological tumor biomarkers in real clinical tests.

研究领域: 分析化学 · 医学诊断 · 癌症研究
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Food Analytical Methods · 2016 ·Vol. 9 ·期 12 ·3501-3508 · IF 2.167

ICP-MS Determination of Potential Toxic Elements in Soil and Rice (Oryza sativa L.) and Related Health Risk

Shao Yufang,Chen Ying,Liu Jian,Wu Pingping,Ying Yibin,Xie Jing

High-resolution inductively coupled plasma mass spectrometry (ICP-MS) was applied to determine potential toxic element pollution in rice and paddy soil in a lead-acid battery production area. The contamination levels of chromium (Cr), cadmium (Cd), and lead (Pb) in rice and soil at three sampling areas were determined, and the uptake mechanism of Cr, Cd, and Pb from soil to rice grain was preliminarily analyzed. The results show that the range of potential toxic elements in rice concentrations is 3.914–11.788, 0.057–1.215, and 0.187–1.585 mg kg −1 for Cr, Cd, and Pb, respectively. For the paddy soils, Cd concentration is 0.610 mg kg −1 , which exceeds 0.300 mg kg −1 , a value recommended by Chinese Environmental Quality. Bioaccumulation factor (BAF, an index of the ability of plant to absorb a particular metal with respect to its concentration in the soil substrate) values of Cr, Cd, and Pb were less than 1 in all rice samples, suggesting that the bioavailability of these metals was relatively low in rice. The correlations between BAF values with organic matter (OM) and pH were calculated to find the mobility and availability of potential toxic elements in soil. At last, the estimated daily intake (EDI) dose was determined to evaluate the health risk to local population via consumption of rice contaminated with Cr, Cd, and Pb. This study indicated that the accumulation and translocation of potential toxic elements from soil to rice could cause the health risk for the local population.

CAS / MDL: 7697-37-2 7601-90-3
研究领域: 环境科学 · 农业化学 · 毒理学 · 公共卫生
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ANALYTICAL LETTERS · 2024 · IF 1.6

Simultaneous Determination of Ultra-Trace Pt, Pd, Rh, and Ir in Gold Mining Residue by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) with an Antimony-Copper Fire Assay and Microwave Digestion

Chunli Fan,Mingying Cao,Qiuju Zheng,Youfa Cheng,Ping Wang,Jinyu Feng

The evaluation of the flow direction of platinum group elements (PGEs) during gold-copper ore mining is challenging due to the uneven distribution and low content. Therefore, it is vital to accurately and simultaneously determine ultra-trace PGEs Pt, Pd, Rh, and Ir in gold mining residue samples. In this study, a method to simultaneously determine ultra-trace Pt, Pd, Rh, and Ir in gold mining residue is reported using Sb–Cu fire assay, microwave digestion, and inductively coupled plasma-mass spectrometry (ICP-MS). The Sb–Cu fire assay was used to enrich Pt, Pd, Rh, and Ir, obtaining Sb–Cu alloy particles that concentrate these elements. An optimal microwave method was employed to digest the Sb–Cu alloy particles. In ICP-MS, the collision reaction interface was used to eliminate the interferences of other elements and improve the accuracy. Moreover, the matrix-matched multi-external standards combined with internal standard calibration were utilized to reduce the error. High concentrations of Au, Ag, and Pb showed no interferences with Pt, Pd, Rh, or Ir determination. The limits of detection for Pt, Pd, Rh, and Ir were 0.018, 0.052, 0.064, 0.035 ng·g−1, respectively, and the relative standard deviation was 5.18, 4.66, 1.55, and 3.17%. Additionally, the determination of Pt, Pd, Rh, and Ir in standard reference materials showed good agreement with the certified values. In summary, a reliable and efficient method is provided to determine various PGEs which is of great significance for gold-copper ore mining.

研究领域: 分析化学 · 矿物加工工程 · 地质学
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Food & Function · 2021 ·Vol. 12 ·期 19 ·8899-8906 · IF 5.396

Elucidating metal ion-regulated flavour formation mechanism in the aging process of Chinese distilled spirits (Baijiu) by electrochemistry, ICP-MS/OES, and UPLC-Q-Orbitrap-MS/MS

Qing Zheng,Yaru Hu,Ayuan Xiong,Ying Su,Zihao Wang,Kun Zhao,Yougui Yu

Elucidating the organometallic interactions in Baijiu will promote a deeper understanding of the flavour formation mechanism during Baijiu aging. However, the organometallic interactions during aging are difficult to explore because the concentration and status of metals in Baijiu samples are affected by other substances (such as organic acids), and the concentrations of these substances also change dynamically. Hence, the flavour formation mechanism of aged Baijiu was investigated based on a multi-method analysis (i.e. electrochemistry, ICP-MS/OES, and UPLC-Q-Orbitrap-MS/MS), which enabled us to solve the difficulty above. The key finding is that, in the aging period, the organic acids induce the transformation of the metal ion state from the complex state to the free state. As a result, the flavour compound (i.e. the esters) contents in aged Baijiu are regulated by the free metal ion-catalyzed reactions.

研究领域: 食品科学 · 分析化学 · 金属有机化学
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FOOD CHEMISTRY · 2019 · IF 5.399

Development and application of a HPLC-ICP-MS method to determine selenium speciation in muscle of pigs treated with different selenium supplements

Kai Zhang,Xiaoqing Guo,Qingyu Zhao,Yunsheng Han,Tengfei Zhan,Ying Li,Chaohua Tang,Junmin Zhang

Dietary selenium deficiency is recognized as a global problem. Pork is the most widely consumed meat throughout the world and an important source of selenium for humans. In this study, a reliable approach was developed for analyzing selenium and its speciation in the muscles of pigs after different selenium treatments. The selenium source deposition efficiency was ranked as: selenomethionine > methylselenocysteine > selenite, and the muscle selenium content had a dose effect with selenomethionine supplementation. In total, four species of selenium were detected in the muscles of pigs and the distributions of these selenium species were greatly affected by the dietary selenium supplementation forms and levels. Selenomethionine (>70% of total selenium) and selenocystine (>11%) were the major selenium species, followed by methylselenocysteine and selenourea. Therefore, selenium-enriched pork produced from selenomethionine is a good source for improving human dietary selenium intake.

CAS / MDL: 2832-45-3
研究领域: 分析化学 · 营养学 · 动物科学
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