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JOURNAL OF RADIOANALYTICAL AND NUCLEAR CHEMISTRY · 2017 ·Vol. 315 ·期 1 ·103-110 · IF 1.282

Rapid method for accurate determination of actinides (U, Th, Pu and Am) in water samples for emergency response

Wang Zhongtang,Lin Jinxian,Li Sixuan,Guo Qiuju,Huang Wenna,Wen Wei,Dan Guiping,Tan Zhaoyi

To rapidly assess the contamination of actinides in emergency water, a method was developed to simultaneously analyze U, Th, Pu and Am. The method consists of two steps: extraction chromatographic separation using UTEVA and DGA resins and isotopic determination of actinides by inductively coupled plasma mass spectrometry (ICPMS). The whole analytical procedure takes only 8 h and high chemical recoveries of actinides were obtained. The cross spectral interferences between actinides in ICPMS measurement were sufficiently removed. The accuracy was validated by analyzing IAEA-443 seawater sample. The low limits of detection of actinides allow this method to distinguish low level contamination.

研究领域: 环境科学 · 核化学
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ANALYTICAL CHEMISTRY · 2021 · IF 6.986

Isotopic Analysis by Laser Ablation Solution Sampling MC-ICP-MS─An Example of Boron

Xiuhong Liao,Zhaochu Hu,Wen Zhang,Yantong Feng,Tao Luo,Zaicong Wang,Ming Li,Keqing Zong,Yongsheng Liu,Shenghong Hu

Using boron as a test analyte, laser ablation (LA) solution sampling multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) is proposed and validated as a fast method for isotopic analysis in natural liquids and digested samples without any prior purification process. We demonstrated that the solution reference standard can be used as a bracketing standard for in situ δ11B analysis in solids. Based on a sensitivity enhancement of 8- to 9-fold, all testing solutions were diluted in a 5% (v/v) NH3·H2O instead of classical 2% (v/v) HNO3. With a discrete and minimal sample solvent loading by the LA sampling strategy, it produces nearly “dry” plasma conditions that tolerate the sample matrix remarkably. The memory effect, one of the most difficult challenges in boron analysis, was dramatically eliminated with only 15 s wash time; thus, each analysis took less than 100 s. No significant matrix effects were observed for varying 50–100% boron concentrations in the samples and varying 20–60% NH3·H2O matrix used for the dilution, as well as for samples doped with a 1/100 synthetic seawater matrix. The external precision of δ11B measurements in NIST 951a was ± 0.30‰ (2SD). Good agreement with the values described in literature studies was achieved for δ11B measurements in eight geological reference materials, with precisions between 0.4 and 0.7‰ (2SD), confirming the accuracy of the proposed method. The proposed method offers advantages of simple sample preparation, fast analysis, and little use of chemical reagents.

研究领域: 地球化学 · 分析化学
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Chinese Herbal Medicines · 2014 · IF 0

Rapid Analysis of Polar Components in Ophiocordyceps sinensis by Conventional Liquid Chromatography System

Wen-qing Li,Wen-jia Li,Zheng-ming Qian,Shi-lin Chen,Li Xiang

Objective To develop a rapid high-performance liquid chromatography coupled with diode array detection (HPLC-DAD) method for the simultaneous determination of six polar compounds in Ophiocordyceps sinensis. Methods A poroshell SB Aq column (50 mm × 4.6 mm, 2.7 μm) and gradient elution were used; The detection wavelength of compounds was set at 260 nm. The chromatographic peaks of the six investigated compounds in sample were identified by comparing their retention times with reference compounds. Results All calibration curves showed good linearity ( r > 0.999) within the tested ranges. The intra- and inter-day precisions of the six analytes were less than 0.8% and 2.1%, respectively, and the recoveries of the six analytes were between 95% and 103%. The validated method was successfully applied to the determination of six polar compounds in O. sinensis samples. Conclusion The poroshell SB Aq column is suitable for the rapid analysis of polar components in Chinese materia medica on conventional HPLC system and the developed HPLC method is also helpful to the quality control of O. sinensis .

CAS / MDL: 64-18-6
研究领域: 中药学 · 分析化学
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ANALYTICAL CHEMISTRY · 2020 · IF 6.785

Rapid Monitoring Approach for Microplastics Using Portable Pyrolysis-Mass Spectrometry

Xiangnan Zhang,Hong Zhang,Kai Yu,Na Li,Yuning Liu,Xiangyu Liu,Hengnan Zhang,Bin Yang,Wenhai Wu,Jing Gao,Jie Jiang

Microplastics (MPs) pollution has drawn increasing concern due to its widespread occurrence and potential risks in the environment. The reliable methods and instruments for fast analysis of microplastics (MPs) less than 5 mm are urgently needed. In this study, a new method based on custom-made portable pyrolysis-mass spectrometry (Pyr-MS) is developed, which enables rapid identification and mass related quantification of MPs. MPs are decomposed in the compact pyrolyzer and then directly analyzed in the portable MS by the chemical fingerprints of polymers including characteristic ions and their special ratio. It avoids the complex extraction and separation procedures of the pyrolysis/thermogravimetric–gas chromatography–mass spectrometry (Pyr/TGA-GC-MS), realizes the rapid analysis of MPs in 5 min, and thus can practically apply to a large number of MPs samples. In comparison to Fourier transform infrared spectroscopy (FT-IR) and Raman, this method is not limited by the shape, size, and color of MPs. Four common plastics including polyethylene (PE), polypropylene (PP), polystyrene (PS), and poly(methyl methacrylate) (PMMA) were investigated to verify the feasibility of this method. The environmental MPs samples collected from a beach were successfully identified and quantified, demonstrating the simplicity and practicality of this approach. The influence of plastics aging on the chemical fingerprints and the potential of mixed plastics detection by Pyr-MS are also assessed. The portable Pyr-MS could provide a promising tool for in-field analysis of MPs such as ship-based marine MPs surveys.

研究领域: 环境科学 · 分析化学
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RSC Advances · 2020 ·Vol. 10 ·期 7 ·4103-4109 · IF 3.119

Exploiting the native inspiratory ability of a mass spectrometer to improve analysis efficiency

Qian Zhang,Lin Lin,Quan Yu,Xiaohao Wang

In this study, a new approach to perform self-aspirating sampling in mass spectrometry (MS) analysis was developed by using the native inspiratory ability of a mass spectrometer. Specifically, the inspiratory channel and sampling inlet of the MS instrument were integrated into a single pathway through a sealed ionization chamber to facilitate analyte delivery and improve sample utilization. Based on this approach, combined with structural simplification and optimization, a versatile electrospray ionization (ESI) source has been constructed and characterized using different mass spectrometers. In addition to the self-aspirating ability, this source configuration can provide sub-ambient pressure (SAP) conditions for ionization, which were conducive to suppressing the background ions generated from some air-involved reactions. Moreover, it can also be used directly for electrospray-driven extraction ionization. With the SAP-ESI source, a conventional mass spectrometer enables rapid analysis of both volatiles and solutions via secondary electrospray ionization and coaxial electrospray ionization, respectively. As the compact gas pathway of the source will promote the efficient transfer and ionization of the sampled substances, the total consumption of the analyte for each analysis can be reduced to subnanogram level and a subppbv limit detection is achieved. Other demonstrated features such as the versatility, easy operation as well as simple assembly will likely contribute to the prevalence of the proposed sampling and ionization strategy.

研究领域: 分析化学 · 质谱技术
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CHROMATOGRAPHIA · 2018 ·Vol. 81 ·期 4 ·669-675 · IF 1.401

Rapid Analysis of Fatty Acid Composition in Polysorbate 80 by Gas Chromatography with On-line Pyrolytic Methylation Technique

Huang Zhongping,Qiu Ruofeng,Huang Yilei,Liu Huijun,Pan Zaifa,Wang Lili

A novel method of on-line pyrolytic methylation–gas chromatography was developed for the rapid analysis of fatty acid composition in Polysorbate 80 without any tedious pre-treatment steps. Fatty acids in Polysorbate 80 were converted into their corresponding fatty acid methyl esters in the presence of trimethylsulfonium hydroxide with a vertical microfurnace pyrolyzer at 300 °C. The premixing procedure of sample and organic alkali reagent was necessary before the on-line pyrolytic methylation to improve the repeatability. The relative standard deviations for peak areas of fatty acids in Polysorbate 80 were over the range of 0.3–9.1% ( n  = 5). Six Polysorbate 80 samples, consisting of three samples of pharmaceutical grade and three samples of non-pharmaceutical grade, were analyzed to evaluate the feasibility of the proposed method. The relative percentages (%) of fatty acids for samples of pharmaceutical grade meet the Chinese Pharmacopoeia requirements with the amount of oleic acid varying from 78.4 to 89.3%. On the other hand, the relative percentages (%) for palmitic acid and stearic acid in samples of non-pharmaceutical grade were out of the specification limits, with the amount of oleic acid varying from 62.0 to 63.5%. The quantitative results determined by on-line pyrolytic methylation were in agreement with those obtained by off-line methylation. The result proved that gas chromatography with on-line pyrolytic methylation technique is of great value for rapid screening analysis of Polysorbate 80 samples in bulks.

研究领域: 分析化学 · 药学
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ANALYST · 2013 ·Vol. 138 ·期 9 ·2598-2603 · IF 3.969

Combination of solid phase extraction and surface-enhanced Raman spectroscopy for rapid analysis

Yongchao Lai,Jingcheng Cui,Xiaohong Jiang,Sha Zhu,Jinhua Zhan

A surface-enhanced Raman spectroscopy (SERS)-active extraction column based on propanethiol modified silver dendrites was fabricated. The column, which combines the advantages of solid phase extraction and SERS, may facilitate the development of rapid analysis with high reliability and accuracy. High temporal stability (under a continuous and intensive laser radiation) and excellent repeatability (repeated extraction and elution) were also achieved using this column. As an example, the quantitative analysis of fluoranthene was accomplished in the concentration range of 0.01–100 μg mL−1 with this column. The extraction process could be accomplished in 10 s and the total time of one sample analysis including extraction, spectral acquisition, elution and intermediate process could be less than 30 s. This method can greatly simplify the sample preparation and reduce the total analysis time.

研究领域: 分析化学 · 环境科学
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RAPID COMMUNICATIONS IN MASS SPECTROMETRY · 2024 ·Vol. 38 ·期 11 ·e9742 · IF 1.8

High-resolution multi-reflection time-of-flight mass spectrometer with atmospheric pressure interface

Shuxiong Yan,Yi Ren,Qi Huang,Yi Hong,Zhengge Chen,Mei Li,Bin Hu,Zhengxu Huang

Rationale Atmospheric pressure interface multi-reflection time-of-flight mass spectrometry (API-MRTOF-MS) has the potential to be a rapid and high-resolution analytical tool for versatile applications in chemistry, biology, environmental science, and medicine. Methods The ions were reflected in a mass analyzer via electrostatic mirrors and folded flight path. Therefore, flight distances were significantly increased. The ion flight path of the API-MRTOF-MS was extended from meters to over 1 km, and the mass resolution was increased. Furthermore, the mass analysis could be completed at around 10 ms due to the rapid response of TOF-MS. Results A high-resolution API-MRTOF-MS approach is successfully developed in this study. The mass resolution could achieve 116 050 (full widths at half maximum [FWHM]) for Cs + ions using an atmospheric pressure electrospray ionization within a total TOF of only 18 ms. An ion transmission efficiency of over 50% was achieved after 600 cycles. Conclusions The analytical performance of the newly developed API-MRTOF-MS demonstrated that it is suitable for high resolution and rapid analysis in many fields.

研究领域: 分析化学 · 质谱技术 · 环境科学 · 医学
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BIOMEDICAL CHROMATOGRAPHY · 2016 ·Vol. 30 ·期 8 ·1331-1337 · IF 1.729

A novelty strategy for the fast analysis of sulfonamide antibiotics in fish tissue using magnetic separation with high-performance liquid chromatography–tandem mass spectrometry

Jincheng Li,Huan Liu,Jing Zhang,Yang Liu,Lidong Wu

A simple, fast and low-cost extraction method with high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS) determination was developed on sulfonamide antibiotics (SAs) in fish tissue. Magnetic separation was first introduced into the rapid sample preparation procedure combined with acetonitrile extraction for the analysis of SAs. Partitioning was rapidly achieved between acetonitrile solution and solid matrix by applying an external magnetic field. Acetonitrile solution was collected and concentrated under a nitrogen stream. The residue was redissolved with 1‰ formic acid aqueous solution and defatted with n- hexane before analysis. The recoveries of SAs were in the range of 74.87–104.74%, with relative standard deviations <13%. The limits of quantification and the limits of detection for SAs ranged from 5.0 to 25.0 μg kg−1 and from 2.5 to 10.0 μg kg−1 , respectively. The presented extraction method proved to be a rapid method which only took 20 min for one sample preparation procedure. Copyright © 2016 John Wiley & Sons, Ltd.

CAS / MDL: 1317-61-9
研究领域: 分析化学 · 环境科学 · 食品安全
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ANALYTICA CHIMICA ACTA · 2022 · IF 6.911

Direct coupling in-tube solid-phase microextraction with mass spectrometry using polymer coated open-tubular column for rapid analysis of antiepileptic drugs in biofluids

Wei Hu,Wei Zhou,Chenlu Wang,Zichun Liu,Zilin Chen

Development of high-throughput and rapid screening analytical method is in high demand for anti-doping and clinical point-of-care (POC) analysis. Solid-phase microextraction and mass spectrometry direct coupling (SPME-MS) has been proved as a rapid and effective way for target analysis in complex sample matrixes. An online direct coupling of in-tube SPME (IT-SPME) with MS using polymer coated open-tubular column has been developed in this work. A sharp stainless-steel needle was attached at the end of the SPME column, which enables the direct ionization of the analytes after elution from the IT-SPME column. Itaconic acid-benzene co-polymer was in-situ grown on the inner surface of the fused silica capillary and used as extraction phase. This column has low backpressure and provides both hydrophobic and weak cationic exchange interaction with the target analytes due to the chemical properties. The developed online IT-SPME-MS method showed good extraction performance towards various target analytes and good reusability at least for 60 times. As a proof-of-concept application, the above method was applied for the analysis of antiepileptic drugs (AEDs) in both plasma and urine samples with linear range (1 ng/mL-200 ng/mL), good linearity (R 2  ≥ 0.99), and good reproducibility (intra-day RSDs less than 4.36%, inter-day RSDs less than 6.55%). The method exhibited high enrichment factors between 187 and 204 for the two AEDs and high sensitivity for the analysis of human plasma samples and urine samples.

研究领域: 分析化学 · 临床医学 · 药物分析
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ANALYST · 2015 ·Vol. 140 ·期 16 ·5662-5670 · IF 4.107

Magnetic solid phase extraction coupled with desorption corona beam ionization-mass spectrometry for rapid analysis of antidepressants in human body fluids

Di Chen,Hao-Bo Zheng,Yun-Qing Huang,Yu-Ning Hu,Qiong-Wei Yu,Bi-Feng Yuan,Yu-Qi Feng

Ambient ionization techniques show good potential in rapid analysis of target compounds. However, a direct application of these ambient ionization techniques for the determination of analytes in a complex matrix is difficult due to the matrix interference and ion suppression. To resolve this problem, here we developed a strategy by coupling magnetic solid phase extraction (MSPE) with desorption corona beam ionization (DCBI)-mass spectrometry (MS). As a proof of concept, the pyrrole-coated Fe3O4 magnetic nanoparticles (Fe3O4@Ppy) were prepared and used for the extraction of antidepressants. After extraction, the Fe3O4@Ppy with trapped antidepressants was then directly subjected to DCBI-MS analysis with the aid of a homemade magnetic glass capillary. As the MSPE process is rapid and the direct DCBI-MS analysis does not need solvent desorption or chromatographic separation processes, the overall analysis can be completed within 3 min. The proposed MSPE-DCBI-MS method was then successfully used to determine antidepressants in human urine and plasma. The calibration curves were obtained in the range of 0.005–0.5 μg mL−1 for urine and 0.02–1 μg mL−1 for plasma with reasonable linearity (R2 > 0.951). The limits of detection of three antidepressants were in the range of 0.2–1 ng mL−1 for urine and 2–5 ng mL−1 for plasma. Acceptable reproducibility for rapid analysis was achieved with relative standard deviations less than 19.1% and the relative recoveries were 85.2–118.7%. Taken together, the developed MSPE-DCBI-MS strategy offers a powerful capacity for rapid analysis of target compounds in a complex matrix, which would greatly expand the applications of ambient ionization techniques with plentiful magnetic sorbents.

研究领域: 分析化学 · 药物分析 · 医学检测
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RSC Advances · 2014 ·Vol. 4 ·期 90 ·49190-49197 · IF 3.708

Microwave-assisted derivatization for fast and efficient analysis of saccharides on disposable microchips

Jinxiu Guo,Shenghong Yang,Xianglu Peng,Fengyun Li,Lei Zhou,Qiaosheng Pu

For rapid and low-cost determination of saccharides with microchip electrophoresis, a domestic microwave oven was used to perform the derivatization of saccharides with 8-aminonaphthalene-1,3,6-trisulfonate (ANTS) for laser-induced fluorescence detection with a 405 nm laser diode. The influence of the reaction conditions was systematically examined. Derivatization of xylose, glucose and lactose was fulfilled within 3 min under the optimized condition. With appropriate selection of the separation medium, these model analytes could be resolved within 30 s in borate solutions containing hydroxypropyl cellulose using disposable cyclic olefin copolymer microchips. Theoretical plate numbers of 1.0 × 106 m−1 and limits of detection of 0.15–0.23 μM were achieved. Peak areas were linear up to 1000 μM for all analytes. The applicability of the proposed method was verified by the determination of glucose in human urine and serum. Separation of oligosaccharides from konjac powder was also demonstrated. The domestic microwave oven, the cheap laser diode and disposable microchips used here make the method an economical way for rapid analysis of saccharides.

CAS / MDL: 5398-34-5
研究领域: 分析化学 · 生物化学
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