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TALANTA · 2020 · IF 5.339

Derivatization assisted LC-p-MRM-MS with high CID voltage for rapid analysis of brassinosteroids

Na An,Quan-Fei Zhu,Lei Yu,Yong-Ting Chen,Sheng-Li Chen,Yu-Qi Feng

In this study, a derivatization-assisted pseudo -multiple reaction monitoring with high CID voltage (HV- p -MRM) strategy was proposed for the analysis of brassinosteroids (BRs) by liquid chromatography-triple quadrupole mass spectrometry (LC-QqQ MS). The concept of the HV- p -MRM strategy was proposed on the basis of an assumption that the precursor ion of analyte is stable in collision cell and less prone to fragmentation at high CID voltage, while co-existing ions (impurity) of easy fragmentation can break down into smaller fragment ions. In such case, by increasing the CID voltage, the co-existing ions that are introduced due to the low resolution of the quadrupole 1 (Q1) can be filtered out by quadrupole 3 (Q3), while the stable precursor ion of analyte will pass through Q3, thereby that the signal-to-noise ratio (S/N) of the analysis can be improved. As a proof-of-concept study, BRs were derivatized with rhodamine B-boronic acid (RhB-BA) and then the derivatives were used to investigate their variations in MS signal, background noise, and S/N upon the CID voltage and MS scanning resolution. The results showed that S/N of these derivatives can be improved in HV- p -MRM mode. To further demonstrate the feasibility of HV- p -MRM strategy, a RhB-BA derivatization assisted LC-HV- p -MRM-MS method was developed for the analysis of BRs. Using this method, rapid and sensitive determination of BRs in different organs of rape flower was achieved. It can be expected that HV- p -MRM may be suitable for the analytes that are stable or can be converted into compounds of high stability in collision cell at high CID voltage.

CAS / MDL: 25895-60-7
研究领域: 植物学 · 分析化学
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Clinical Implant Dentistry and Related Research · 2019 ·Vol. 21 ·期 2 ·324-335 · IF 3.212

A thermosensitive chitosan-based hydrogel for sealing and lubricating purposes in dental implant system

Xiaoxiao Cao,Xinjie Cai,Ruiying Chen,Huimei Zhang,Tao Jiang,Yining Wang

Background Mechanical and biological complications associated with implant systems happen frequently in the clinic. Purpose To develop a chitosan (CS)-based thermosensitive hydrogel for sealing and lubricating purposes in dental implant system. Materials and Methods In this study, a thermosensitive hydrogel made up of CS, β-glycerophosphate pentahydrate (β-GP), and povidone-iodine (PVP-I), called CS/β-GP/PVP-I thermosensitive hydrogel, was fabricated. Three experimental groups with different volume ratios of CS to β-GP were prepared, namely 16/4, 13/7, and 10/10 groups. The surface topography of the different groups and their physicochemical characteristics were examined by SEM, FTIR, and X-ray diffraction analysis. The cytotoxicity of the hydrogel was examined by CCK-8 test. In vitro antibacterial efficiency was analyzed by the spread plate method. Sealing ability was detected by incubating two-piece implants in Escherichia coli suspension. Lubricating ability of the hydrogel was evaluated by the removal torque test with a calibrated digital torque meter. Results The CS/β-GP/PVP-I thermosensitive hydrogel was fabricated and showed a highly porous structure under SEM. An in vitro cytotoxicity test demonstrated that 13/7 group displayed no cytotoxicity. Furthermore, all three groups showed obviously antibacterial effects. In the sealing ability test, 16/4 group showed the best sealing ability. The removal torque of 16/4 group and 13/7 group was significantly greater than control group. Conclusions Based on our findings, it could be concluded that the thermosensitive and antibacterial CS/β-GP/PVP-I hydrogel with sealing and lubricating ability was successfully prepared. The hydrogel had better sealing and lubricating effects when the volume ratio of CS to β-GP was 16/4.

CAS / MDL: 25655-41-8
研究领域: 牙科学 · 生物材料 · 生物医学工程
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JOURNAL OF THE AMERICAN SOCIETY FOR MASS SPECTROMETRY · 2016 · IF 3.031

Characteristics of Ion Activation and Collision Induced Dissociation Using Digital Ion Trap Technology

Fuxing Xu,Qiankun Dang,Xinhua Dai,Xiang Fang,Yuanyuan Wang,Li Ding,Chuan-Fan Ding

Collision induced dissociation (CID) is one of the most established techniques for tandem mass spectrometry analysis. The CID of mass selected ion could be realized by ion resonance excitation with a digital rectangular waveform. The method is simple, and highly efficient CID result could be obtained by optimizing the experimental parameters, such as digital waveform voltage, frequency, and q value. In this work, the relationship between ion trapping waveform voltage and frequency at preselected q value, the relationship between waveform frequency and the q value at certain ion trapping voltage for optimum CID efficiency were investigated. Experiment results showed that the max CID efficiency of precursor reserpine ions can be obtained at different trapping waveform voltage and frequency when q and β are different. Based on systematic experimental analysis, the optimum experimental conditions for high CID efficiency can be calculated at any selected β or q. By using digital ion trap technology, the CID process and efficient fragmentation of parent ions can be realized by simply changing the trapping waveform amplitude, frequency, and the β values in the digital ion trap mass spectrometry. The technology and method are simple. It has potential use in ion trap mass spectrometry.

CAS / MDL: 50-55-5
研究领域: 分析化学 · 质谱学
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JOURNAL OF MASS SPECTROMETRY · 2023 ·Vol. 59 ·期 1 ·e4990 · IF 2.3

Does deprotonated benzoic acid lose carbon monoxide in collision-induced dissociation?

Yingying Liu,Xue Wang,Danyang Zhang,Chen Wang,Haijiao Xie,Hongping Chen,Yunfeng Chai

Decarboxylation is known to be the major fragmentation pathway for the deprotonated carboxylic acids in collision-induced dissociation (CID). However, in the CID mass spectrum of deprotonated benzoic acid ( m/z 121) recorded on a Q-orbitrap mass spectrometer, the dominant peak was found to be m/z 93 instead of the anticipated m/z 77. Based on theoretical calculations, 18 O-isotope labeling and MS 3 experiments, we demonstrated that the fragmentation of benzoate anion begins with decarboxylation, but the initial phenide anion ( m/z 77) can react with trace O 2 in the mass analyzer to produce phenolate anion ( m/z 93) and other oxygen-containing ions. Thus oxygen adducts should be considered when annotating the MS/MS spectra of benzoic acids.

研究领域: 分析化学 · 质谱学
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2026 · IF 4.1

Synergistic integration of μ-SPE and ammoniated adduct-based MRM for sensitive UPLC-MS/MS quantification of PEG1000: a comparative study against in-source CID and application to zebrafish tissue distribution

Zhou Xinyue,Duan Sufei,Lou Yuye,Deng Yue,Feng Shuang,Liu Jiale,Zhang Jiarui,Xi Yalin,Shi Meiyun,Yin Lei

A sensitive UPLC-MS/MS method was developed and validated for quantifying polyethylene glycol 1000 (PEG1000) in zebrafish tissues, featuring a systematic comparison of two MS acquisition strategies. Through comprehensive optimization, the ammonium adduct [M+NH 4 ] + of the representative 18-EO oligomer ( m/z 828.5) was selected as the precursor ion, achieving approximately fourfold higher signal intensity than [M+H] + . Critically, the conventional high declustering potential in-source CID approach monitoring fragment ions was outperformed by the optimized MRM method monitoring the intact ammoniated precursor, which demonstrated 2.7-fold signal enhancement and superior selectivity. The integration of micro-solid-phase extraction (μ-SPE) further improved method performance, yielding 1.5-fold signal gain and markedly reduced matrix effects compared to conventional protein precipitation. The fully validated method exhibited excellent linearity (0.5–50 μg/mL, r  > 0.995), accuracy, precision, and stability. Application to zebrafish tissue distribution studies revealed pronounced organ-specific accumulation following aqueous exposure to 200 μg/mL PEG1000, with highest concentrations in intestine tissue exhibiting a time-dependent increase, followed by muscle, while muscle maintained consistently low levels. This analytical platform, synergistically combining μ-SPE cleanup and ammoniated adduct-based MRM, offers superior sensitivity over in-source CID approaches and provides a practical framework for polymer bioanalysis, yielding critical insights into the in vivo fate of PEG-based compounds. The key novelties of this work are the following: (i) the first systematic comparison between ammoniated adduct MRM and high-DP in-source CID for PEG1000 quantification; (ii) the introduction of μ-SPE for sample preparation in zebrafish tissues, achieving 1.5-fold signal enhancement; and (iii) the successful application of this platform to reveal organ-specific accumulation patterns of PEG1000. Graphical abstract

CAS / MDL: 25322-68-3 64-18-6
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