Analytical Methods
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2025
·
IF 2.6
Ning Wang,Siyu Xie,Peng Liu,Leting Wang,Chao Zhong,Jun Yu,Manman Qin,Huanwen Chen
Semen Platycladi is a widely used natural product in Chinese medicine with pharmacological effects such as anti-arteriosclerosis, sleep improvement, antioxidant and anti-inflammatory. The quality of Semen Platycladi is fundamentally important for its therapeutic use. However, tedious sample pretreatment required by the currently available methods poses great challenge to the high throughput analysis and evaluation of the quality of Semen Platycladi. Here we established a high-throughput analysis platform for evaluating the quality of various Semen Platycladi samples using Internal Extractive Electrospray Ionization Mass Spectrometry (iEESI-MS). The fatty acids including linoleic acid, linolenic acid, arachidonic acid, stearic acid and palmitic acid, known as one of the major ingredients in Semen Platycladi, were directly quantified in the range of 0.001-100.00 μg/mg (R2 > 0.995) using raw samples of different origins, with the limits of detection of 0.02 - 0.04 μg/mg, the limits of quantification of 0.07 - 0.14 μg/mg, the recovery rate of 89.5 - 102.0%, and the relative standard deviation of repeatability (n=9) of 0.51% - 3.88%, respectively. The data revealed that these five fatty acids were the main differential compounds, which could be used to differentiate the samples originated from Hebei, Shandong and Henan province. The experimental results demonstrated that the iEESI-MS could be a useful platform for fast quality analysis of Semen Platycladi, and thus showing advanced applications in natural product analysis, drug discovery and related fields.
研究领域:
中药学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
RAPID COMMUNICATIONS IN MASS SPECTROMETRY
·
2012
·Vol. 26
·期 7
·719-727
·
IF 2.79
Yingzhi Liu,Bo Su,Xian Wang
RATIONALE The study of interactions between protein and pharmaceutical molecules including natural extracts has become of increasing interest in biological and biomedical research. An investigation of the interaction between saikosaponins and cytochrome c (Cyt c) by electrospray ionization mass spectrometry (ESI-MS) is described in this study. Saikosaponins are found in Bupleurum falcatum (a flowering plant), and they are glycosides that consist of saccharides and the sapogenins of triterpenoids. METHODS Seven model molecules of saccharides and triterpenes, namely maltose (Mal II), maltotriose (Mal III), raffinose (Raf), and stachyose (Sta), glycyrrhetinic acid (Gly), ursolic acid (Urs) and oleanic acid (Ole), were chosen to perform a series of ESI-MS control experiments for the exploration of the interaction groups in saikosaponins with Cyt c. The dissociation constants of detected noncovalent complexes were determined by using a direct ESI-MS assay. RESULTS We have observed in the ESI mass spectra the formation of Cyt c complexes with saikosaponins a and c, and these saccharides, with 1:1 and 1:2 stoichiometry. Our results showed that no complex ions of triterpenes and Cyt c were detected in the ESI-MS and similar Kd values were obtained for the Cyt c complexes of saikosaponins and saccharides. This demonstrates that the glycosyl moiety in the saikosaponins is the effective interaction group with Cyt c. We propose that saikosaponins and saccharides interact with Cyt c by hydrogen bonds. The binding affinity of these six ligands with Cyt c is shown to be in the order Ssa > Ssc > Raf, Mal III > Sta ≥ Mal II. CONCLUSIONS The ESI-MS methodology presented in this study enables us to investigate the interactions of saikosaponins with Cyt c, and allows the direct determination of binding constants. These results could guide further research for providing insights into the structure-binding relationship of ligands with Cyt c. Copyright © 2012 John Wiley & Sons, Ltd.
研究领域:
生物化学
·
药物学
✓ 已验证
DOI
高影响因子
JOURNAL OF ETHNOPHARMACOLOGY
·
2021
·
IF 4.36
Zi-Dong Qiu,Xiaoping Zhang,Xu-Ya Wei,Konstantin Chingin,Jia-Quan Xu,Wei Gao,Bin Yang,Shuang-Long Wang,Ting Tan,E-Hu Liu,Hai-Yu Xu,Guang-Hong Cui,Juan Guo,Ya-Nan Wang,Ye Shen,Yu-Jun Zhao,Huan-Wen Chen,Chang-Jiang-Sheng Lai,Lu-Qi Huang
Ethnopharmacological relevance Aconitum carmichaelii Debeaux, a famous traditional medicinal herb for collapse, rheumatic fever , and painful joints, always raises global concerns about its fatal toxicity from toxic alkaloids when improperly processed. Therefore, it is urgent to clarify the internal molecular mechanism of processing detoxification on Aconitum and develop simple and reliable approaches for clinical application, which is also of great significance to the rational medicinal use of Aconitum . Aim of the study The study aimed at developing a complete molecular mechanism exploration strategy in complex medicinal herb decocting system, clarifying the internal molecular mechanism of processing detoxification on Aconitum, and exploring valid approaches for detoxification. Materials and methods Aconiti Lateralis Radix Praeparata (Fuzi) was selected as the model for exploring the complex Aconitum detoxification mechanism using an advanced online real-time platform based on extractive electrospray ionization mass spectrometry. The methods realized the sensitive capture of dynamic trace intermediates, accurate qualitative and quantitative analysis, and real-time and long-term monitoring of multi-components with satisfactory accuracy and resistance to complex matrices. Results Components in the complex Aconitum decocting system were real-timely characterized and fat meat was discovered and verified to directionally detoxify Aconitum while reserving the therapy effect. More importantly, the dynamic detoxification mechanism in the chemically complex Aconitum decoction was molecularly profiled. A novel reaction pathway based on nucleophilic substitution reaction mechanism was proposed. As confirmed by the theoretic calculations at DFT B3LYP/6-31G (d) levels, fatty acids ( e.g. , palmitic acid) acted as a green, cheap, and high-performance catalyst and promote the decomposition of toxic diester alkaloids to non-toxic and active benzoyl-monoester alkaloids through the discovered mechanism. Conclusion The study exposed a novel detoxification molecular mechanism of Aconitum and provided an effective method for the safe use of Aconitum , which could effectively guide the development of traditional processing technology and compatibility regulation of the toxic herb and had great value to the modernization and standardization development of traditional medicine.
研究领域:
民族药理学
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中药学
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分析化学
✓ 已验证
DOI
PubMed
高影响因子
JOURNAL OF THE AMERICAN SOCIETY FOR MASS SPECTROMETRY
·
2014
·
IF 3.193
Konstantin Chingin,Ning Xu,Huanwen Chen
The charge states of biomolecular ions in ESI-MS can be significantly increased by the addition of low-vapor supercharging (SC) reagents into the spraying solution. Despite the considerable interest from the community, the mechanistic aspects of SC are not well understood and are hotly debated. Arguments that denaturation accounts for the increased charging observed in proteins sprayed from aqueous solutions containing SC reagent have been published widely, but often with incomplete or ambiguous supporting data. In this work, we explored ESI MS charging and SC behavior of several biopolymers including proteins and DNA oligonucleotides. Analytes were ionized from 100 mM ammonium acetate (NH4Ac) aqueous buffer in both positive (ESI+) and negative (ESI–) ion modes. SC was induced either with m-NBA or by the elevated temperature of ESI capillary. For all the analytes studied we, found striking differences in the ESI MS response to these two modes of activation. The data suggest that activation with m-NBA results in more extensive analyte charging with lower degree of denaturation. When working solution with m-NBA was analyzed at elevated temperatures, the SC effect from m-NBA was neutralized. Instead, the net SC effect was similar to the SC effect achieved by thermal activation only. Overall, our observations indicate that SC reagents enhance ESI charging of biomolecules via distinctly different mechanism compared with the traditional approaches based on analyte denaturation. Instead, the data support the hypothesis that the SC phenomenon involves a direct interaction between a biopolymer and SC reagent occurring in evaporating ESI droplets.
研究领域:
分析化学
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生物物理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ENVIRONMENTAL AND EXPERIMENTAL BOTANY
·
2020
·
IF 4.027
Shangguang Du,Meng Cui,Yali Cai,Ahui Xue,Yingbin Hao,Xueyong Huang,Lihua Liu,Liping Luo
Chilling stress is a major production threat for rice ( Oryza sativa L.). The mechanism of chilling response has not been unveiled up to now, especially at the metabolomic level. In this study, two Asian rice cultivars, Qiutianxiaoting (chilling-tolerant variety) and 93−11 (chilling-susceptible variety), were used to analyze the metabolic changes when exposed to low temperature and recovered by extractive electrospray ionization mass spectrometry (EESI-MS). Physiological and metabolic analysis combining with bioinformatics were performed to reveal cold resistance mechanism of these two varieties. Physiological analysis showed that only Qiutianxiaoting survived after 36 h chilling treatment, and the growth indexes of Qiutianxiaoting took on a decreasing trend, but these indexes of 93−11 appeared a trend of increase under cold treatment; moreover, the levels of antioxidant activities (SOD, POD and CAT) were higher in Qiutianxiaoting than 93−11, especially at recovery stage. PCA and OPLS-DA analysis all showed that Qiutianxiaoting, not 93−11, could be separated with each other under chilling stress, which indicated that these two subspecies of rice had different mechanisms to resist cold temperature. The results of metabolic analysis indicated that low temperature activated phenylpropanoid biosynthesis and flavone and flavonol biosynthesis in 93−11, while it induced the expression of methyl jasmonate biosynthesis-related genes in Qiutianxiaoting, which might mitigate chilling damage and effectively make it more cold-resistant than 93−11. This study would shed some lights on the cold resistance mechanism of these two rice cultivars in terms of physiological and metabolic analysis.
研究领域:
植物学
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农学
✓ 已验证
DOI
高影响因子
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
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2024
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IF 5.7
Hongda Wang,Lili Hong,Feifei Yang,Yuying Zhao,Qi Jing,Wei Wang,Min Zhang,Yang Yang,Qinhua Chen,Ying Hu,Yadan Zou,Xue Li,Wenzhi Yang
Ginsenosides and lipids are both bioactive ingredients for ginseng. Targeting these two categories of components, this study was designed to develop desorption electrospray ionization-mass spectrometry imaging approaches and spatial metabolomics strategies, achieving the visualization and differentiation among different parts of Panax ginseng root (e.g., rhizome, main root, lateral root, fibrous root, and adventitious root). Potential chemical markers were identified by searching an in-house ginsenoside library and online Lipid Maps database, together with high-resolution MS2 data analysis. Six ginsenosides and 11 lipids were diagnostic to differentiate five different parts of the P. ginseng root. Additionally, three ginsenosides and 20 lipids were identified as differential markers among the six positions of the main root of P. ginseng. High-abundance malonyl- and oleanolic acid-ginsenosides were observed in the rhizome. These results assist in understanding the accumulation of bioactive molecules all through the root of P. ginseng, which can benefit its quality control and rational use.
研究领域:
植物化学
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分析化学
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中药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF RADIOANALYTICAL AND NUCLEAR CHEMISTRY
·
2014
·Vol. 302
·期 1
·575-581
·
IF 1.415
Dai Ying,Zhang Anyun
A new supermolecular recognition agent named tetra - tert -butyl-calix[4]-bis[(4-methly-1,2-phenylene-crown-6] ( Tert ButylCalixC) was synthesized. Batchwise experiments of extraction of Na(I), K(I), Rb(I), Cs(I), Sr(II), Ba(II), Ru(III) and Fe(III) from aqueous solution with Tert ButylCalixC/ o -nitroanisole were carried out. Effects of HNO 3 concentration, contact time and temperature on the extraction behavior were examined. The equilibrium established within 30 min implied a fast extraction kinetics. The optimal operation temperature was 298 K. Stoichiometry of Tert ButylCalixC and Cs(I) by electrospray ionization mass spectrometry characterization revealed 1:1 molar ratio. It was observed that the extraction system of Tert ButylCalixC/ o -nitroanisole was effective for selective removal of Cs(I), showing remarkable separation performance.
研究领域:
化学
·
环境科学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2019
·
IF 3.858
Hengqing Fu,Cheng Qian,Wenjun Tong,Huihui Li,David D.Y. Chen
Affinity capillary electrophoresis (ACE) in a free solution must be used to confirm the molecular interaction observed in electrospray ionization mass spectrometry (ESI-MS) for affinity binding analysis in the drug discovery process. In this article, the affinity of ibuprofen with three cyclodextrin species of different cavity sizes is investigated by both ESI-MS and ACE methods. Because the binding interactions are measured in different environments using ESI-MS (gas phase) and ACE (liquid phase), the experimental results show significant differences. To better illustrate the major factors influencing the binding constants in different environments, two types of simulations (molecular docking and molecular force field evaluation) are employed in the theoretical discussion. The molecular docking results were consistent with the ESI-MS experimental phenomena. Due to lack of the water molecules in the gas phase, a substantial difference in molecular interaction can contribute to a different binding affinity. By using the molecular modeling based on the force field evaluation with considering solvent molecules, β-CD is expected to form the most stable complex with ibuprofen in the liquid phase and the binding affinity of ibuprofen to γ-CD is much less significant than it is in gas phase. This prediction is in good agreement with the ACE results. Therefore, this work demonstrates that, by using ESI-MS in the first-step screening and ACE in the follow-up determination, a more accurate understanding can be achieved.
研究领域:
药物化学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
CHEMICAL RESEARCH IN TOXICOLOGY
·
2025
·
IF 3.8
Qiaoyun Huang,Jianfeng Zhang,Songbin Dong,Bin Hu
Medical swabs are commonly used in routine medical sampling and testing of human body fluids, such as saliva and sputum. Many medical swabs are made of plastic polymers. Exposure to plastic medical swabs containing many free soluble polymers and residual monomers could increase the potential health risk. Conventional analytical methods for assessing personal exposure to polymers usually require complex sample preparation and time-consuming analytical procedures. In this study, we established a direct electrospray ionization mass spectrometry method to investigate the occurrence and species of soluble polymers in different medical swabs. The migration of typical soluble polymers, i.e., PA6 and PEG, was found in medical swabs and human saliva after swabbing within seconds. The amounts of PA6 and PEG were found to be nanograms per swab. Trace polymer could rapidly reside in saliva within seconds (e.g., 3 s). The exposure level of polymer residual was evaluated during different swabbing times and saliva volumes, showing the concentration of soluble polymers in saliva at the ng/mL level. Despite the low concentration and low toxicity of soluble polymers in saliva, it is anticipated that this method could offer a convenient and simple way to evaluate polymer exposures rapidly. We also hope our findings will attract more attention to the health risks of ubiquitous plastic materials in daily life and propose an efficient strategy to eliminate saliva polymers.
研究领域:
医学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL BIOCHEMISTRY
·
2022
·
IF 3.191
Mingying Ma,Tianhao Wu,Gongwei Sun,Sichun Zhang
Monitoring clinical biomarkers, such as testosterone in serum, is important for disease assessment. Due to the very low concentration of testosterone in serum, we have developed a new strategy for its enrichment in serum samples by magnetic molecularly imprinted polymers (MMIPs) technology and detection by nano-electrospray ionization mass spectrometry (Nano-ESI-MS). Testosterone was selectively extracted and enriched by the imprinted polymers on the surface of magnetic particles and the complex matrix was eliminated from the serum. The linear calibration curve was in the range of 0.1–10 μg/L and the limit of detection was 11.4 ng/L. The recovery and repeatability of the spiked serum were satisfactory. These results demonstrate that the proposed method is a promising approach for quantitative analysis of testosterone in serum.
研究领域:
分析化学
·
临床医学
·
生物医学工程
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL LETTERS
·
2017
·
IF 1.15
Li-Ping Luo,Teng-Hui Yu,Xing-Xing Liu,Xue-Yong Huang,Xiao-Wei Fang,Xing-Lei Zhang,Xia-Li Guo
Neutral desorption-extractive electrospray ionization mass spectrometry was used for the direct, rapid, and quantitative determination of chlorpyrifos in honey without pretreatment. Under the optimized conditions, the limit of detection was 1.64 ng/mL with a linear dynamic range from 10 to 1,000 ng/mL and relative standard deviations from 1.97 to 6.14%. The recoveries of fortified honey samples at 50 and 500 ng/mL were 82.02 and 109.28% with relative standard deviations of 4.02 and 4.34%, respectively. This protocol offers high sensitivity, good precision, rapid analysis, and high specificity in a complex matrix.
研究领域:
分析化学
·
食品科学
✓ 已验证
产品关联
DOI
高影响因子
RSC Advances
·
2017
·Vol. 7
·期 82
·52091-52100
·
IF 3.108
Yanying Huang,Yanfang Ma,Huawen Hu,Pengran Guo,Lei Miao,Yunyun Yang,Min Zhang
In this study, a molecularly imprinted polymer-coated wooden-tip (MIPCWT) electrospray ionization mass spectrometry (ESI-MS) method was developed for rapid and sensitive detection of trace malachite green (MG) and its metabolite in aquatic products. Such a method was realized by applying a silicone-modified acrylate molecularly imprinted emulsion (SMAMIE) onto the surface of wooden tips to specially design a MIPCWT solid-phase micro-extraction (SPME) probe for selective enrichment of MG and its metabolite from aquatic products. Subsequently, a high voltage and some spray solvent were applied to the MIPCWT SPME probe, and ESI was induced for direct MS analysis under ambient and open-air conditions. The MIPCWT-SPME probe exhibits a high enriching capacity of approximately 1500–2000 fold toward MG and leucomalachite green (LMG), with detection limit reaching 0.01 μg L−1. In addition, a good linearity is obtained for both MG and LMG, with correlation coefficient values (R2) of no less than 0.998. The present method was successfully applied to analyze MG and LMG in real-life tap water, river water and fish samples, and good recoveries in the range of 93–103%, 92–108% and 106–113%, respectively, were found. All of these demonstrated that our developed MIPCWT-ESI-MS method holds great potential for rapid, direct, sensitive, and reliable detection and analysis of trace veterinary drug residues in aquatic products.
研究领域:
分析化学
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食品安全
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环境科学
✓ 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）