JOURNAL OF THE ELECTROCHEMICAL SOCIETY
·
2020
·Vol. 167
·期 12
·126506
·
IF 3.721
Tingting Hao,Chunfeng Zhang,Han Lin,Wenting Wei,Fan Yang,Yangbo Wu,Lingmei Niu,Weijun Kang,Zhiyong Guo
Herein, a dual-mode aptasensor for subnanomolar detection of lead ions Pb2+ based on electrochemiluminescence (ECL) and fast scan voltammetry (FSV) was developed. It could be one-step fabricated using an all-in-one probe Fe3O4@Au-ssDNA&Ru-NH2 which has multiple functions: Fe3O4 core achieves one-step preparation of the aptasensor; Au shell provides a place for assembly and electrochemical reactions; ssDNA can selectively recognize and capture target Pb2+, and ferrocene labeled on it could provide fast scan voltammetric signal and participate in changes of ECL signals; and Ru-NH2 is a signal marker for ECL detection. In presence of target Pb2+, ssDNA folds to form G-quadruplex, and ferrocene labeled on its end approaches to the Au shell surface resulting in easier electron transfer. So the electrochemical signal is enhanced, and ECL quenching occurs. Electrochemical peak current increased about 1000 times at 100 V s−1 using FSV, making its sensitivity compatible with that of ECL to obtain highly sensitive dual-mode detection. Pb2+ could be detected in the concentration range from 10−10 mol l−1 to 10−6 mol l−1 with a limit of quantitation (LOQ) 10−10 mol l−1. Selectivity, stability, reproducibility, accuracy and practicality are good. This extremely simple method provides a valuable idea for developing biosensors for field detection applications.
研究领域:
分析化学
·
生物传感技术
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产品关联
DOI
高影响因子
CHEMOMETRICS AND INTELLIGENT LABORATORY SYSTEMS
·
2016
·
IF 2.217
Zhi Liu,Hai-Long Wu,Li-Xia Xie,Yong Hu,Huan Fang,Xiao-Dong Sun,Tong Wang,Rong Xiao,Ru-Qin Yu
Mycotoxins are a class of highly carcinogenic substances often naturally occurring in the moldy foods especially cereals. In the present work, a smart chemometrics-assisted analytical strategy that combines liquid chromatography-full scan-mass spectrometry (LC-MS) detection with second-order calibration method based on alternating trilinear decomposition (ATLD) algorithm is developed for direct, fast and interference-free determination of multi-class regulated mycotoxins in complex cereal samples with one-step ultrasound-assisted extraction. Ten mycotoxins with different property are fast eluted out (9.0 min) under a simple gradient LC-separation and detected by full scanning MS with a segmented fragment program. With the aid of prominent "second-order advantage" of the algorithm, the problems of co-eluted peaks, unknown interferences and baseline drifts occurring in the LC-MS profiles are mathematically resolved, making "pure signals" of targeted analytes can be extracted out from heavily interferential information. The new strategy avoids intricate physical/chemical clean-up steps to significantly improve the accuracy of the trace analysis of mycotoxins, average recoveries of ten analytes in both complex cereal samples (maize and rice) range from 93.8 to 109% with standard deviations (SD) lower than 9.8%, and the limits of detection (LOD) range from 0.01 to 1.17 μg kg −1 . In order to further confirm the reliability of the method, the same batch of samples is analyzed using LC-MS 2 method with complicated immunoaffinity column (IAC) purification step, the elliptical joint confidence region (EJCR) tests of quantitative results of ten mycotoxins show that higher precision is obtained using the proposed method. Therefore, this new strategy can be as an attractive alternative for simple, fast and accurate determination of multi-class mycotoxins in complex cereal samples.
研究领域:
食品科学
·
分析化学
✓ 已验证
DOI
高影响因子
ANALYTICA CHIMICA ACTA
·
2021
·
IF 6.558
Fengming Xiao,Huiqian Zhou,Han Lin,Hongze Li,Tinglang Zou,Yangbo Wu,Zhiyong Guo
In this work, a novel fast scan digital circuit for voltammetric analysis with precious ohmic drop compensation is developed, which is achieved through online measuring solution resistance first and then proportionally feedbacking the output signal to potentiostat's in-phase input through a potentiometer. It mainly consists of a solution resistance measurement module based on AD5933 chip, an ohmic drop automatic compensation module and a STM32F103ZET6 microcontroller. The performance of the circuit is checked successively using pure resistances, RC dummy cells, RC dummy cells incorporating a pseudo-faradaic component, and the ferrocene redox system . Results show that, precise ohmic drop compensation can be realized online and automatically, affording fast scan cyclic voltammetric (FSCV) analysis for theoretical electrochemical cells at 2000 V/s and that for practical electrochemical system using conventional electrodes at 1600 V/s. Based on this circuit, a very simple DNA biosensor for ultrasensitive detection of mercuric ions was explored. Benefitting from the high sensitivity brought by the high scan rate, the limit of quantitation (LOQ) can reach 1 pmol/L, demonstrating the application potential of FSCV in the field of ultrasensitive electrochemical detection .
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Shuai Ji,Xian Shao,Zhen-yu Su,Lei Ji,Yu-jie Wang,Yun-su Ma,Lu Zhao,Yan Du,Meng-zhe Guo,Dao-quan Tang
Fufang Danshen Dripping Pill (FDDP) and Clopidogrel Bisulfate Tablet (CBT) are usually combined for treatment of coronary artery diseases in clinical. To investigate the pharmacokinetic interaction between FDDP and CBT after oral administration of FDDP, CBT and their combination in rats, a novel LC–MS method with segmented scan modes (multiple reaction monitoring and selected ion monitoring) and polarity (positive and negative ionization) was developed. Clopidogrel and the main active ingredients of FDDP, with different chemical and ionization properties, were simultaneously quantified in plasma in a single run. The method was validated in terms of specificity, linearity, precision, accuracy, recovery, matrix effect and stability. As a result, co-administration of FDDP and CBT significantly altered the pharmacokinetic parameters of danshensu, ginsenoside Rb1, dihydrotanshinone I, tanshinone I and tanshinone IIA of FDDP, as well as clopidogrel. Mechanism studies suggested that induction of liver cytochrome P450 isozymes CYP2C11 and CYP3A1 by co-administration, as well as inhibition of carboxyl esterase 1, was partly responsible for FDDP-CBT pharmacokinetic interactions. The developed LC–MS method could be used to simultaneously quantify different types of in vivo analytes in a single run, and the results could be used for clinical medication guidance of FDDP and CBT.
研究领域:
药理学
·
分析化学
·
药学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF ALLOYS AND COMPOUNDS
·
2017
·
IF 3.133
Yi Yang,Shifeng Wen,Qingsong Wei,Wei Li,Jie Liu,Yusheng Shi
The TiAl/TiB 2 metal matrix composites (MMCs) are fabricated by selective laser melting (SLM), and the effects of scan line spacing on the grains feature, crystallographic texture, phases evolution mechanism and nanohardness have been systematic studied. With the increase of scan line spacing, relatively coarse grains with average grain size of 4.9 ± 0.2 μm and strong ( 0001 ) orientation gradually transforms into refined grains with average grain size of 4.2 ± 0.1 μm and dominated ( 11 2 ¯ 1 ) and ( 01 1 ¯ 1 ) orientations during the SLM process. The SLM-processed TiAl/TiB 2 MMCs samples are dominated by high-angle grain boundaries (HAGBs) and α 2 phase, with the increase of scan line spacing from 80 μm to 140 μm, both the volume fraction of HAGBs and α 2 phase decrease. During the SLM process, the phases evolution mechanism of TiAl/TiB 2 MMCs can be expressed as: (200)β first transformed to (11 2 ¯ 0)α 2 , (20 2 ¯ 0)α 2 and (110)γ, then the TiB 2 , residual B 2 and incompletely transformed γ phases randomly distribute in the α 2 matrix, and the orientation relationship of the α 2 , γ, B 2 and TiB 2 phases can be concluded as: ( 11 2 ¯ 0 ) α 2 // ( 110 ) B 2 // ( 110 ) γ// ( 110 ) TiB 2 . Besides, there are some TiB phase in the TiAl/TiB 2 MMCs which is induced by the Ti + TiB 2 → 2TiB reaction during SLM. The TiAl/TiB 2 MMCs samples show an ultra-high nanohardness ranging from 8.6 ± 0.4 GPa to 9.4 ± 0.5 GPa with the increase of scan line spacing, which is superior than that of the TiB 2 reinforced TiAl alloy counterpart (6.7 ± 0.4 GPa) fabricated by traditional roll bonding.
研究领域:
材料科学
·
力学
✓ 已验证
产品关联
DOI
高影响因子
ANALYTICA CHIMICA ACTA
·
2020
·
IF 5.977
Xiao-Dong Sun,Hai-Long Wu,Jun-Chen Chen,An-Qi Chen,Yue Chen,Yang-Zi Ouyang,Yu-Jie Ding,Ru-Qin Yu
A novel soft strategy for combination and partition of mass spectra data recorded at different fragmentor voltages in full scan mode of a mass spectrometer was developed to generate abundant multi-way data. It is the first time that non-linear four-way and combined three-way LC-MS data have been obtained simultaneously in a single chromatographic run. This strategy ensures that each analyte can be ionized and detected at the most appropriate MS conditions (ionization modes, fragmentor voltages) and avoids a hard chromatographic segmentation in subsequent chemometric analysis. Two different experimental datasets were analyzed to validate the feasibility and applicability of this strategy. Some simple pretreatments were carried out before LC-MS analysis to prevent potential matrix effects. Proper chemometric tools were used to resolve three-way (partitioned data) and enhanced three-way LC-MS (combined data) data, respectively. The method was assessed by comparing the analytical results obtained from the same chemometric algorithm with both combined and partitioned datasets: (1) the combined data provided the best global overall resolution, higher sensitivity and more reliable results, (2) the partitioned data provided higher selectivity for some specific analytes. The results showed that the developed method could be a soft and ingenious tool to handle the unordered but information-rich raw LC-MS data. Moreover, the proposed strategy could take extra analytical advantages in terms of higher sensitivity and more reliable quantitative results when compared with LC-MS (with single fragmentor voltage) strategy and showed nearly the same capability in analytical quality as classic LC-MS/MS method.
研究领域:
分析化学
·
生物信息学
✓ 已验证
DOI
高影响因子
MOLECULES
·
2018
·Vol. 23
·期 10
·2496
·
IF 3.098
Ying Zhou,Jian Guan,Weiwei Gao,Shencong Lv,Miaohua Ge
In this research, fifteen carbamate pesticide residues were systematically analyzed by ultra-high performance liquid chromatography–quadrupole-linear ion trap mass spectrometry on a QTRAP 5500 system in both multiple reaction monitoring (MRM) and enhanced product ion (EPI) scan modes. The carbamate pesticide residues were extracted from a variety of samples by QuEChERS method and separated by a popular reverse phase column (Waters BEH C18). Except for the current conformation criteria including selected ion pairs, retention time and relative intensities from MRM scan mode, the presence of carbamate pesticide residues in diverse samples, especially some doubtful cases, could also be confirmed by the matching of carbamate pesticide spectra via EPI scan mode. Moreover, the fragmentation routes of fifteen carbamates were firstly explained based on the mass spectra obtained by a QTRAP system; the characteristic fragment ion from a neutral loss of CH3NCO (−57 Da) could be observed. The limits of detection and quantification for fifteen carbamates were 0.2–2.0 μg kg−1and 0.5–5.0 μg kg−1, respectively. For the intra- (n =3) and inter-day (n =15) precisions, the recoveries of fifteen carbamates from spiked samples ranged from 88.1% to 118.4%, and the coefficients of variation (CVs) were all below 10%. The method was applied to pesticide residues detection in fruit, vegetable and green tea samples taken from local markets, in which carbamates were extensively detected but all below the standard of maximum residue limit.
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DOI
高影响因子
EUROPEAN JOURNAL OF MASS SPECTROMETRY
·
2019
·
IF 0.851
Shencong Lv,Henghui Wang,Yong Yan,Miaohua Ge,Jian Guan
A simple, rapid, and efficient liquid chromatography tandem mass spectrometry (LC–MS/MS) method, operated in electrospray ionization and quadrupole linear ion trap modes, has been developed for the identification and structural characterization of aflatoxins in peanuts and its derivative products or bean sauce. Samples (5 g) were extracted with acetonitrile/water/formic acid (79:20:1, v/v). After centrifugation and dilution, the extracts were separated on a C18 analytical column by gradient elution (acetonitrile/0.2% formic acid) and analyzed by UPLC–MS/MS. External calibration was used for qualification. The developed multiple reaction monitoring–information-dependent acquisition–enhanced product ion method enabled quantification and confirmation of the analytes in a single run. Enhanced product ion mode was used for qualitative analysis, while multiple reaction monitoring mode was used for quantitative analysis. An in-house library was constructed for identification. Calibration curves showed good linearity with correlation coefficients (r) higher than 0.994. Limits of detection were determined to be below 0.26 µg kg−1 for most analytes. The recoveries for those substances were in the acceptable range of 80.2%–119.1%. A new LC–MS3 method was established for further confirmation. One pickled pepper peanut was found to contain aflatoxins B1, B2, and G1 with contents of 90.93, 26.64, and 1.92 µg kg−1, respectively.
研究领域:
食品安全
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2015
·Vol. 8
·期 3
·666-672
·
IF 1.821
L. Chen,Y. Qin,X. Yang,C. Liu
An analytical method for the simultaneous determination of seven insecticides, including six neonicotinoids and one pyridine-azomethine, in drinks by LC-MS/MS using the Product Ion Confirmation Scan (PICS) mode was developed and validated. The compounds were extracted by modified QuEChERS and purified by d-SPE. The separation of all compounds was achieved in less than 3 minutes using a BEH C18 reverse-phase column and a mobile phase composed of 0.01% formic acid in water and methanol in the gradient elution mode at 0.4 mL min−1. Except for the two transitions and retention time demanded by EU/2002, identification was further carried out by matching the mass spectrum between the reference and sample produced by PICS if necessary. The LODs and LOQs for all compounds were lower than 0.014 μg L−1 and 0.05 μg L−1, respectively. The calibration curves were ranging from the LOQ to 0.02 mg L−1 with r2 higher than 0.9917 and reasonable recoveries were between 81.19% and 105.79% with RSD <15.0%. This work illustrates the advantages of using the PICS mode to build MRM acquisition methods in the application field of pesticide multi-residue analysis. It is very effective when only one MRM transition is obtained or the confirmation ion transition is too weak. It is proved that this is a rapid and reliable analytical method.
研究领域:
食品科学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
CHEMOMETRICS AND INTELLIGENT LABORATORY SYSTEMS
·
2016
·
IF 2.217
Hui-Wen Gu,Hai-Long Wu,Shan-Shan Li,Xiao-Li Yin,Yong Hu,Hui Xia,Huan Fang,Ru-Qin Yu,Peng-Yuan Yang,Hao-Jie Lu
In this work, a rapid chemometrics-enhanced liquid chromatography–single stage mass spectrometry (LC–MS) was developed for the simultaneous green determination of six co-eluted sulfonylurea-type oral antidiabetic agents (SOADs) in health teas and human plasma samples. Shortening the chromatographic separation time and reducing the cost per analysis were achieved via using full scan mode of LC–MS under simple isocratic elution condition followed by an environment-friendly “mathematical separation” strategy. The problem of the complete separation of target analytes from each other and/or from the uncalibrated interferences in complex matrices was resolved by alternating trilinear decomposition (ATLD) method as a posteriori . Satisfactory qualitative and quantitative results were obtained even in the existence of unknown interferences and the “second-order advantage” was fully exploited. The average spiked recoveries for all target analytes were between 81.6% and 110.1% with standard deviations less than 7.7%. It was demonstrated that the proposed strategy could be promisingly used for green resolution and determination of co-eluted multi-analytes of interest in complex samples while avoiding elaborate sample pretreatment steps and complicated experimental conditions as well as more sophisticated high-cost instrumentations.
研究领域:
分析化学
·
药物分析
·
质谱分析
·
色谱分析
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产品关联
DOI
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 10
·e4306
·
IF 1.688
Jie Yang,Zhi Sun,Duolu Li,Fei Duan,Zhuolun Li,Jingli Lu,Yingying Shi,Tanye Xu,Xiaojian Zhang
Shenkang injection is a traditional Chinese formula with good curative effect on chronic renal failure. In this paper, a novel, rapid and sensitive ultra-high-performance liquid chromatography coupled with Q Exactive hybrid quadrupole Orbitrap high-resolution accurate mass spectrometry was developed and validated for simultaneous determination of seven bioactive constituents of Shenkang injection in rat plasma and tissues after intravenous administration. Acetonitrile was used as a protein precipitation agent in biological samples disposal with carbamazepine as internal standard. The chromatographic separation was carried out on a C 18 column with a gradient mobile phase consisting of acetonitrile and water (containing 0.1% formic acid). The MS analysis was performed in the full-scan positive and negative ion mode. The lower limits of quantification for the seven analytes in rat plasma and tissues were 0.1–10 ng/mL. The validated method was successfully applied to tissue distribution and pharmacokinetic studies of Shenkang injection after intravenous administration. The results of the tissue distribution study showed that the high concentrations of seven constituents were primarily in the kidney tract. This is the first report of the application of Q-Orbitrap with full-scan mass spectrometry in tissue distribution and pharmacokinetic studies of Shenkang injection.
研究领域:
中药学
·
分析化学
·
药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2014
·
IF 4.517
Hui-Wen Gu,Hai-Long Wu,Xiao-Li Yin,Yong Li,Ya-Juan Liu,Hui Xia,Shu-Rong Zhang,Yi-Feng Jin,Xiao-Dong Sun,Ru-Qin Yu,Peng-Yuan Yang,Hao-Jie Lu
β-blockers are the first-line therapeutic agents for treating cardiovascular diseases and also a class of prohibited substances in athletic competitions. In this work, a smart strategy that combines three-way liquid chromatography–mass spectrometry (LC–MS) data with second-order calibration method based on alternating trilinear decomposition (ATLD) algorithm was developed for simultaneous determination of ten β-blockers in human urine and plasma samples. This flexible strategy proved to be a useful tool to solve the problems of overlapped peaks and uncalibrated interferences encountered in quantitative LC–MS, and made the multi-targeted interference-free qualitative and quantitative analysis of β-blockers in complex matrices possible. The limits of detection were in the range of 2.0 × 10 −5 –6.2 × 10 −3 μg mL −1 , and the average recoveries were between 90 and 110% with standard deviations and average relative prediction errors less than 10%, indicating that the strategy could provide satisfactory prediction results for ten β-blockers in human urine and plasma samples only using liquid chromatography hyphenated single–quadrupole mass spectrometer in full scan mode. To further confirm the feasibility and reliability of the proposed method, the same batch samples were analyzed by multiple reaction monitoring (MRM) method. T -test demonstrated that there are no significant differences between the prediction results of the two methods. Considering the advantages of fast, low-cost, high sensitivity, and no need of complicated chromatographic and tandem mass spectrometric conditions optimization, the proposed strategy is expected to be extended as an attractive alternative method to quantify analyte(s) of interest in complex systems such as cells, biological fluids, food, environment, pharmaceuticals and other complex samples.
研究领域:
分析化学
·
医学检验
·
药物分析
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）