Journal of Analytical Methods in Chemistry
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2024
·
IF 2.3
Yajie Hao,Guang Yin,Xuemei Wang,Juan Fu,Qihui Cao,Qinyong Sun,Guimin Zhang,Zhong Feng
Rosuvastatin calcium is a widely used 3-hydroxy-3-methylglutaryl coenzyme A-reductase inhibitor developed for the treatment of dyslipidemia. To establish a control strategy for the elemental impurities, a new digestion method combined with an inductively coupled plasma-mass spectrometer (ICP-MS) was developed and validated by our team to determine elements Cd, Pb, As, Hg, Co, V, and Ni in rosuvastatin calcium tablets, which digest the sample perfectly even in the presence of a large number of excipients, especially titanium dioxide. The measurement mode was collision cell mode with kinetic energy discrimination (KED). 209Bi+, 115In+, and 89Y+ were chosen as internal standard elements. The recoveries of the limit of quantitation (LOQ) ranged from 90.5% to 106.4%, concentrations of the abovementioned elements in LOQ were 0.25 µg·L−1, 0.25 µg·L−1, 0.75 µg·L−1, 1.5 µg·L−1, 2.5 µg·L−1, 5 µg·L−1, and 8 µg·L−1 , respectively, linear correlation coefficients were above 0.9997, the recoveries in accuracy item ranged from 91.8% to 103.6%, and relative standard deviations (RSDs) of recovery in precision were not more than 1.8%, reflecting a reliable method of high sensitivity, strong anti-interference capacity, and good precision, and that it was suitable for the determination of elemental impurities in drugs.
研究领域:
药学
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分析化学
✓ 已验证
DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
·
2023
·
IF 7.4
Rui Yang,Ronggang Zheng,Jiangyun Song,Hao Liu,Sujuan Yu,Jingfu Liu
The application of selenium nanoparticle (SeNP)-based fertilizers can cause SeNPs to enter the soil environment. Considering the possible transformation of SeNPs and the species-dependent toxicity of selenium (Se), accurate analysis of SeNPs and other Se species present in the soil would help rationally assess the potential hazards of SeNPs to soil organisms. Herein, a novel method for speciation of SeNPs and other Se species in soil was established. Under the optimized conditions, SeNPs, selenite, selenate, and seleno amino acid could be simultaneously extracted from the soil with mixtures of tetrasodium pyrophosphate (5 mM) and potassium dihydrogen phosphate (1.2 μM), while inert Se species (mainly metal selenide) remained in the soil. Then, extracted SeNPs can be effectively captured by a nylon membrane (0.45 μm) and quantified by inductively coupled plasma mass spectrometry (ICP-MS). Other extracted Se species can be separated and quantified by high-performance liquid chromatography coupled with ICP-MS. Based on the difference between the total Se contents and extracted Se contents, the amount of metal selenide can be calculated. The limits of detection of the method were 0.02 μg/g for SeNPs, 0.05 μg/g for selenite, selenate, and selenocystine, and 0.25 μg/g for selenomethionine, respectively. Spiking experiments also showed that our method was applicable to real soil sample analysis. The present method contributes to understanding the speciation of Se in the soil environment and further estimating the occurrence and application risks of SeNPs.
研究领域:
环境科学
·
分析化学
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DOI
PubMed
高影响因子
JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY
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2024
·Vol. 39
·期 7
·1938-1947
·
IF 3.1
Lingke Li,Fei Wu,Yongsheng Liu,Tao He,Jie Lin,Wen Zhang,Rui Li,Haihong Chen,Keqing Zong,Zhen Zeng,Zhaochu Hu
Stable nickel (Ni) isotopes have shown great potential for investigating planetary accretion processes, mantle–crust magmatism, and paleo-marine evolution. The development of an economical and time-efficient separation method for Ni isotope analysis holds significant value within the realm of Ni isotope research. Previous purification methods for Ni isotope analysis have typically relied on either multi-column procedures or the utilization of significant quantities of organic reagents, such as acetic acid, acetone, and dimethylglyoxime. In this study, a novel two-column chromatographic separation procedure was presented for the determination of Ni isotope compositions in geological materials. A cation resin (AG50W-X8) was utilized in conjunction with diluted HCl and HF to effectively remove a substantial portion of matrix elements. Subsequently, trace amounts (100–200 μL) of Ni-spec resin were used for further purification of Ni. This relatively simple purification scheme for Ni isotope analysis effectively reduces the use of organic reagents and the amount of Ni-spec resin compared to previous methods that relied on multi-column separation and organic reagent extraction. Ni isotopic compositions were analyzed using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). The instrumental mass discrimination of Ni isotopic ratios was corrected for using the double spike (DS) combined with the sample–standard bracketing (SSB) method. The Ni isotope compositions (δ60Ni) of in-house standards (SCP and CUG) were −0.06 ± 0.05‰ (2 SD, n = 104) and 0.36 ± 0.06‰ (2 SD, n = 97), respectively. Furthermore, the measured δ60Ni values of various geological reference materials (BCR-2, BHVO-2, BIR-1, DTS-1, DTS-2b, SDO-1, GSP-2, and W-2a from the USGS; JB-1b from the GSJ; GSR-2, GSR-3, GSR-4, GSR-5, and GSR-10 from the NRCGA) were consistent with previous studies within measurement error. Additionally, the δ60Ni values of AGV-1 from the USGS, as well as those of GSR-10, GSR-12, GSR-15, GSR-17, GSR-18, and GSR-19 from the NRCGA are reported here for the first time. Based on repeated measurements of pure solutions and reference materials, the long-term reproducibility of δ60Ni values was better than ± 0.06‰ (2 SD). Consequently, our study presents a relatively straightforward purification method for Ni for its isotopic analysis using only trace amounts of organic reagents and Ni-spec resin.
研究领域:
地球化学
·
同位素地球化学
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产品关联
DOI
高影响因子
ANALYTICAL SCIENCES
·
2021
·Vol. 37
·期 12
·1735-1740
·
IF 2.081
Zhao Liangcheng,Wei Li,Hu Yanqiao,Chen Qingzhi,Cheng Wencui,Zhang Jinming,Li Xing,An Ziyi,Meng Jianwei,Liu Huajie
Existing methods can not achieve rapid mass decomposition and multi-element analysis of graphite ore samples. In this study, it is found that molten lithium metaborate can destroy the structure of graphite, causing graphite C to be oxidized and decomposed in an oxygen environment. We have established a method for testing graphite ore samples with lithium metaborate at 950°C with melting–ultrasonic extraction–ICP-AES multi-element (Al, Ca, Fe, K, Mg, Mn, Na, P, Si, and Ti) testing. The verification results of the national first-level reference materials show that the detection limit of this method is low and the accuracy and precision are good. The results of the measured samples show no significant difference between this method and the classical chemical analysis method. This method has the following advantages over the existing ones: simple operation process, faster decomposition and testing, low reagent consumption, reduced possibility of sample contamination, and better results reproducibility.
研究领域:
分析化学
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材料科学
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产品关联
DOI
PubMed
高影响因子
PLoS One
·
2017
·Vol. 12
·期 9
·e0185302
·
IF 2.806
FuKai Li,AiJun Gong,LiNa Qiu,WeiWei Zhang,JingRui Li,Yu Liu,YuNing Liu,HuiTing Yuan
The determination of trace rare-earth elements (REEs) can be used for the assessment of environmental pollution, and is of great significance to the study of toxicity and toxicology in animals and plants. N, N, N′, N′-tetraoctyl diglycolamide (TODGA) is an environmental friendly extractant that is highly selective to REEs. In this study, an analytical method was developed for the simultaneous determination of 16 trace REEs in simulated water samples by inductively coupled plasma optical emission spectroscopy (ICP-OES). With this method, TODGA was used as the extractant to perform the liquid-liquid extraction (LLE) sample pretreatment procedure. All 16 REEs were extracted from a 3 M nitric acid medium into an organic phase by a 0.025 M TODGA petroleum ether solution. A 0.03 M ethylenediaminetetraacetic acid disodium salt (EDTA) solution was used for back-extraction to strip the REEs from the organic phase into the aqueous phase. The aqueous phase was concentrated using a vacuum rotary evaporator and the concentration of the 16 REEs was detected by ICP-OES. Under the optimum experimental conditions, the limits of detection (3σ, n = 7) for the REEs ranged from 0.0405 ng mL -1 (Nd) to 0.5038 ng mL -1 (Ho). The relative standard deviations (c = 100 ng mL -1 , n = 7) were from 0.5% (Eu) to 4.0% (Tm) with a linear range of 4–1000 ng mL -1 (R 2 > 0.999). The recoveries of 16 REEs ranged from 95% to 106%. The LLE-ICP-OES method established in this study has the advantages of simple operation, low detection limits, fast analysis speed and the ability to simultaneously determine 16 REEs, thereby acting as a viable alternative for the simultaneous detection of trace amounts of REEs in water samples.
研究领域:
分析化学
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环境科学
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DOI
高影响因子
JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY
·
2016
·Vol. 31
·期 7
·1391-1399
·
IF 3.379
Jing Zhang,Beibei Chen,Han Wang,Xi Huang,Man He,Bin Hu
Microfluidic devices provide a potential platform that can specialize in miniaturization, integration and automation. In this study, we prepared ethanediamine modified poly glycidyl methacrylate trimethylol propane triacrylate monolithic columns (poly (GMA-co-TRIM-NH2)) in a microfluidic chip channel and established a novel method by combining chip-based poly (GMA-co-TRIM-NH2) monolithic microextraction with inductively coupled plasma mass spectrometry (ICP-MS) for the determination of bismuth in cell samples. Various factors affecting chip-based monolithic microextraction of bismuth were investigated. Under the optimized conditions, the limit of detection was 0.21 ng mL−1 and the relative standard deviation for bismuth was 6.0% (c = 5 ng mL−1, n = 7). The method was successfully applied to the analysis of HepG2 cells incubated with bismuth. With consumption of ∼600 cells, the average amount of bismuth was determined to be at the sub picogram level in a single cell. The prepared chip-based poly (GMA-co-TRIM-NH2) monolithic column had a high-surface area and exhibited high extraction efficiency towards bismuth. The proposed chip-based monolithic microextraction method combined with ICP-MS provides a novel strategy for the analysis of trace metals in cells.
研究领域:
分析化学
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生物技术
·
材料科学
✓ 已验证
产品关联
DOI
高影响因子
GEOSTANDARDS AND GEOANALYTICAL RESEARCH
·
2013
·Vol. 38
·期 3
·345-354
·
IF 2.77
Jie Li,Xi-Rong Liang,Li-Feng Zhong,Xuan-Ce Wang,Zhong-Yuan Ren,Sheng-Ling Sun,Zhao-Feng Zhang,Ji-Feng Xu
en This link goes to a English section fr This link goes to a French section A novel preconcentration method is presented for the determination of Mo isotope ratios by multi-collector inductively coupled plasma-mass spectrometry (MC-ICP-MS) in geological samples. The method is based on the separation of Mo by extraction chromatography using N-benzoyl-N-phenylhydroxylamine (BPHA) supported on a microporous acrylic ester polymeric resin (Amberlite CG-71). By optimising the procedure, Mo could be simply and effectively separated from virtually all matrix elements with a single pass through a small volume of BPHA resin (0.5 ml). This technique for separation and enrichment of Mo is characterised by high selectivity, column efficiency and recovery (~ 100%), and low total procedural blank (~ 0.18 ng). A 100 Mo- 97 Mo double spike was mixed with samples before digestion and column separation, which enabled natural mass-dependent isotopic fractionation to be determined with a measurement reproducibility of < 0.09‰ (δ 98/95 Mo, 2 s ) by MC-ICP-MS. The mean δ 98/95 Mo SRM 3134 (NIST SRM 3134 Mo reference material; Lot No. 891307) composition of the IAPSO seawater reference material measured in this study was 2.00 ± 0.03‰ (2 s , n = 3), which is consistent with previously published values. The described procedure facilitated efficient and rapid Mo isotopic determination in various types of geological samples. en This link goes to a English section fr This link goes to a French section Une nouvelle méthode de pré-concentration est présentée pour la détermination des rapports isotopiques du Mo par spectrométrie de masse à source plasma et multi-collection (MC -ICP-MS) dans des échantillons géologiques. La méthode est basée sur la séparation du Mo par Chromatographie d'extraction en utilisant du N-benzoyle-N- phénylhydroxylamine (BPHA) supporté par une résine polymère d'ester acrylique microporeuse (Amberlite CG- 71). En optimisant la procédure, le Mo peut être simplement et efficacement séparé de la quasi-totalité des éléments de la matrice avec un seul passage à travers un petit volume de résine BPHA (0,5 ml). Cette technique de séparation et d'enrichissement du Mo est caractérisée par une grande sélectivité, une grande efficacité et une grande récupération de la colonne (~ 100%), et un faible total de la procédure de blanc (~ 0,18 ng). Un double spike Mo 100 -Mo 97 a été mélangé avec les échantillons avant la digestion et la séparation sur colonne, ce qui a permis la détermination du fractionnement isotopique naturel dépendant de la masse avec une reproductibilité de mesure de < 0,09 ‰ ( δ98/95 Mo, 2s) par MC -ICP-MS. La composition moyenne δ 98/95 Mo SRM 3134 (matériau de référence NIST SRM 3134 Mo; Lot n ° 891307) de l'eau de mer de référence IAPSO mesurée dans cette étude est de 2,00 ± 0,03 ‰ (2s, n = 3), ce qui est cohérent avec les valeurs précédemment publiées. La procédure décrite facilite une détermination efficace et rapide des rapports isotopiques du Mo dans divers types d’échantillons géologiques.
研究领域:
地球化学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY
·
2020
·Vol. 36
·期 2
·429-438
·
IF 3.498
Ying Zhang,Jianguo Qu,Yan Chang,Yue Li
Phosphorus concentrations in water are usually determined using phosphomolybdenum blue (PMB) spectrophotometry. However, the measurement of extremely low phosphorus concentrations by this method is limited for various reasons. This work systematically developed a highly sensitive analytical method for the measurement of dissolved ultra-trace phosphorus by inductively coupled plasma mass spectrometry with methane mixed plasma (CH4-ICP-MS). We determined the optimal radio frequency (RF) power and verified the sensitizing effect of carbon-containing plasma, showing that the addition of 6.0 mL min−1 methane can significantly improve the sensitivity of phosphorus detection. There was no mass spectral interference in the determination of phosphorus in medium resolution mode. The species of phosphorus, dissolved organic carbon (DOC) concentrations ≤15.0 mg L−1, and salinity ≤3.4 had no effect on the determination of phosphorus. DOC concentrations >15.0 mg L−1 had some inhibitory effect on the determination, but microwave digestion eliminated the effect of organic matter with good reproducibility. Salinity levels >3.4 have an inhibitory effect on the determination and the samples need to be diluted or desalinated for accurate determination. The limit of detection (LOD) for the determination of phosphorus by CH4-ICP-MS is 7.3 ng L−1. The accuracy and precision of this method are 2.5% and 1.3%, respectively. The determination precision values for phosphorus in drinking water and in natural samples such as Arctic glacier meltwater, lake water, river water, seawater and rain water were all within 3.5%, and the spike recovery rates were 101.2–103.8%. The method developed here thus has a low LOD and high accuracy. Using the proposed method, ultra-trace phosphorus in low-phosphorus samples such as polar water can be directly measured, which simplifies the sample pretreatment process, and the sample is not easily contaminated by reagents.
研究领域:
分析化学
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环境科学
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产品关联
DOI
高影响因子
GEOSTANDARDS AND GEOANALYTICAL RESEARCH
·
2020
·Vol. 44
·期 3
·617-627
·
IF 2.976
Ying Yu,Qian Zhao,Haolin Bao,Qing Mou,Zeming Shi,Youliang Chen,Ying Gao
With increasing use of bismuth in industry, a better understanding of its environmental behaviour is required, including an improved knowledge of its background concentration range in (non-saline) freshwaters. However, the poor analytical sensitivity of previous methods may lead to inaccurate measurement results for Bi 3+ in environmental samples. In this work, cobalt ion-assisted photochemical vapour generation (PVG) was developed for the detection of trace Bi with inductively coupled plasma-mass spectrometry (ICP-MS) measurement. The volatile species of Bi was found to be (CH 3 ) 3 Bi generated under UV irradiation in the presence of formic acid, acetic acid and Co 2+ . The major parameters potentially influencing the detection of Bi were investigated. Under optimised conditions, the limit of detection (3 s , n = 11) of the proposed method was 0.3 ng l −1 . The analytical sensitivity was enhanced about 70-fold for Bi 3+ compared with that using classic pneumatic nebulisation of ICP-MS. Furthermore, the proposed method showed better analytical sensitivity and anti-interference ability towards co-existing ions compared with ferric ion-assisted PVG systems. The accuracy of the proposed method was evaluated by analysis of environmental water samples and certified reference materials with satisfactory results.
研究领域:
分析化学
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环境科学
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产品关联
DOI
高影响因子
GEOSTANDARDS AND GEOANALYTICAL RESEARCH
·
2018
·Vol. 42
·期 3
·309-318
·
IF 3.929
Tao He,Junyi Xie,Zhaochu Hu,Ting Liu,Wen Zhang,Haihong Chen,Yongsheng Liu,Keqing Zong,Ming Li
Bromine and iodine are important tracers for geochemical and environmental studies. In this study, a rapid acid digestion (HNO 3 + HF) with ammonia dilution for the simultaneous determination of bromine and iodine in soils and sediments using ICP-MS was developed. The recoveries of Br and I were controlled by the synergic effect of temperature and time. It took only 15 min at 140 °C for the complete recovery of Br and I in sediment (GSD-2) and soil (GSS-24) reference materials, which is a process that needs 2–6 h at 90 °C. A serious loss of Br and I was found at a higher digestion temperature of 190 °C. A 5% v/v NH 4 OH dilution effectively eliminated the memory effects and stabilised the signals of Br and I. Moreover, ammonia dilution also avoided the corrosiveness of HF on the sample introduction system and torch of ICP-MS. Tellurium is a more suitable internal standard element than In in the ammonia medium. To avoid the adsorption of residues of dissolution on Te, addition of Te should be carried out after centrifuging the solution. The developed method was successfully applied to determine Br and I in fifty-three Chinese soil and sediment reference materials. This simple method shows great potential for the rapid determination of Br and I in large batches of geological and environmental samples commonly analysed for mineral exploration and environmental geochemistry studies.
研究领域:
环境科学
·
地球化学
✓ 已验证
产品关联
DOI
高影响因子
Scientific Reports
·
2018
·Vol. 8
·期 1
·1-14
·
IF 4.122
Huang Wenli,Jiao Jie,Ru Mei,Bai Zhenqing,Yuan Honglin,Bao Zhian,Liang Zongsuo
Coptis chinensis Franch. is one of the most important medicinal plants globally. However, this species contains relatively high concentrations of chromium (Cr) which potentially detrimental to human health. It is important to understand Cr localization and speciation in order to evaluate its accumulation and transportation mechanisms and minimize Cr transfer to humans. As little previous work in this area has been carried out, we utilized synchrotron radiation microscopic X-ray fluorescence (SR-μXRF) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) to spatially locate Cr, X-ray absorption near-edge spectroscopy (XANES) to analyze Cr speciation, and inductively coupled plasma mass spectrometry (ICP-MS) to detect Cr subcellular concentration. Micromapping results showed that Cr was distributed predominantly within the vascular cylinder, the periderm and some outer cortex, and the cortex and some vascular bundles in root, rhizome, and petiole, respectively. XANES data showed that Cr(VI) can be reduced to Cr(III) when grown with Cr(VI), and yielded a novel conclusion that this plant contain elemental chromium. ICP-MS data showed that Cr was primarily compartmentalized in cell walls in all tissues. The new insights on Cr accumulation in C. chinensis Franch. provide a theoretical basis for the evaluation of Cr in other medicinal plants.
研究领域:
植物学
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环境科学
·
药用植物研究
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DOI
高影响因子
GEOSTANDARDS AND GEOANALYTICAL RESEARCH
·
2025
·
IF 3.4
Tao He,Hui Cao,Wang Lang,Zhaochu Hu,Zaicong Wang,Zongqi Zou,Wen Zhang,Haihong Chen,Yongsheng Liu
Silver is a powerful geochemical tracer in various geological processes (e.g., hydrothermal deposit formation and evolution of the terrestrial and Martian mantles). The measurement of the ultra-trace Ag (< 0.1 μg g -1 ) in geological samples by ICP-MS is often hindered due to serious polyatomic interferences arising from Zr, Nb and Y elements presented in samples. In this study, a simple and rapid ammonia coprecipitation method was developed to remove interference elements (Zr, Nb and Y) in NH 4 HF 2 digests for the determination of Ag mass fractions in geological materials by isotope dilution ICP-MS (ID-ICP-MS). The removal of interference elements (Zr, Nb and Y) in digestion solutions of geological materials was achieved using ammonia coprecipitation, effectively eliminating their polyatomic interferences. To compensate for the incomplete recovery of Ag during ammonia coprecipitation, isotope dilution calibration was chosen over internal standard calibration to achieve final accurate results. The limit of quantitation for Ag using the proposed method was 1.83 ng g -1 . The results obtained for Ag mass fractionation in nine international geological reference materials were in good agreement with the published values obtained by ID-ICP-MS and ICP-MS/MS. The proposed simple, rapid and practical analytical method for the determination of Ag mass fractions improves our understanding of the behaviour of silver in cosmochemistry and geochemistry studies.
研究领域:
地球化学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）