JOURNAL OF MASS SPECTROMETRY
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2023
·Vol. 59
·期 1
·e4990
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IF 2.3
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
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质谱学
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DOI
PubMed
高影响因子
JOURNAL OF FOOD AND DRUG ANALYSIS
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2021
·
IF 6.079
Wei Jia,Yuyang Liu,Xi Xu,Yanxi Zhang,Lin Shi
A novel magnetic adsorbent solid-phase Fe 3 O 4 @ZIF-8 extraction method coupled with UHPLC Q-Orbitrap high resolution mass spectrometry for the sensitive and high efficiency detection of fluoroquinolones, tetracyclines, dyes and amphenicols in eggs is described. Under optimum conditions, CCβ and CCα of 0.62 to 26.97 μg.kg −1 and 0.36 to 16.37 μg.kg −1 was obtained, which is much better than that obtained by conventional methods. The accuracy, expressed as recovery, were achieved falling between 75% and 104%. The proposed strategy provides several advantages of simplicity and low energy consumption, thus retaining potential for the screening of risky drugs in various samples.
研究领域:
分析化学
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食品安全
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生物医学
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DOI
PubMed
高影响因子
MOLECULES
·
2022
·Vol. 27
·期 9
·2631
·
IF 4.927
Lian Zhu,Shengjun Ma,Kailin Li,Pei Xiong,Shihan Qin,Wei Cai
Arnebiae Radix(dried root ofArnebia euchroma(Royle) Johnst.) has been used in traditional Chinese medicine (TCM) to treat macular eruptions, measles, sore throat, carbuncles, burns, skin ulcers, and inflammation. Previous studies have shown that shikonins and shikonofurans are two of their main bioactive ingredients. However, systematic investigations of their constituents have rarely been conducted. It is necessary to establish a rapid and effective method to identify the chemical constituents ofArnebiae Radix. This will help to further improve the effective resource utilization rate of this plant. In this study, a rapid and effective UHPLC-Q-Exactive Orbitrap mass spectrometry method was established to simultaneously analyze chemical ingredients inArnebiae Radixwithin a short period of time. Based on the results of a full scan MS, the MS2database (mzVault and mzCloud), the diagnostic fragment ions, the retention time, and the bibliography, a total of 188 compounds were identified, with 114 of those being reported fromArnebiae Radixfor the first time. The results of this study lay the foundation for obtaining a thorough understanding of the active ingredients inArnebiae Radixand its quality control. This method may be widely used for the chemical characterization of different samples.Keywords:Arnebiae Radix;identification;chemical constituents;UHPLC-Q-Exactive Orbitrap MS
研究领域:
中药学
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分析化学
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DOI
PubMed
高影响因子
Journal of Chemistry
·
2024
·Vol. 2024
·期 1
·6719888
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IF 2.8
Shihan Qin,Xue Jiang,Shani Li,Qing Li,Jin Huang,Qingjiao He,Wei Cai
The dried root of Sophora davidii Kom. ex Pavol (Leguminosae, family) is a folk medicine and has long been used for the treatment of various diseases, including cough, hematochezia, sore throat, and dysentery. In this study, UHPLC-Q-Exactive Orbitrap mass spectrometry investigations were applied to obtain the profiling of the flavonoids in S. davidii . Finally, 108 compounds were identified, and 85 of them were firstly reported. Then, the in vitro antioxidant activity and tyrosinase activity of S. davidii were investigated using the DPPH radical scavenging ability, hydroxyl radical scavenging, and copper-reducing ability method and by measuring the rate of tyrosinase-catalyzed L-dopa oxidation. To our knowledge, this is the first study of S. davidii’s antioxidant activity, anti-tyrosinase activity, and systematic characterization of flavonoids. The current study will be of support for the usage of S. davidii in the future development of the pharmaceutical industry.
研究领域:
药学
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植物化学
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DOI
高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
·
2025
·
IF 6.6
Xichuang Guo,Keyun Cheng,Chenxin Wang,Jing Zheng,Yeshun Wu,Siwei Wang,Xixi Zeng,Zhujun Mao,Jinyan Gong,Gongshuai Song,Xi Chen,Qing Shen
Fritillaria Bulbus (FB) is a medicinal food homologous substance containing various alkaloids. However, the authenticity and quality control of FB have been regarded as the important and challenging factors in globalization and modernization. In this study, the spatial distributions of alkaloids from four FBs ( Fritillaria thunbergii Miq, FritiLlaria cirrhosa D. Don, Fritillaria ussuriensis Maxim, Fritillaria unibracteata var. wabuensis) were analyzed by a consolidation of UPLC-Q-Extractive Orbitrap MS/MS and direct desorption electrospray mass spectrometry imaging (DESI-MSI). Results showed that 58 reliable metabolites (mainly alkaloids) were identified preliminarily, and taxonomic models were built by chemometric analysis. The alkaloid contents in the bulb base were significantly higher than those in bulb and bulblet ( p < 0.05). Seven metabolites, hexadecanamide, imperialine, L-phenylalanine, jervine, peimine, L-pyroglutamic acid, and trans-3-indolacrylic acid, were screened and confirmed as key characteristic compounds of FB. The detailed spatial information provides a reliable means for rational evaluation of the quality control of FBs. It can better utilize the enriched portion of the alkaloids in FBs. It can provide reference value for the identification of adulteration and development of the medicinal food homologous substance.
研究领域:
药学
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分析化学
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产品关联
DOI
高影响因子
Drug Design Development and Therapy
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2020
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IF 3.216
Xiaofang Jiang,Lin Zhou,Lihua Zuo,Xiaohui Wang,Yingying Shi,Xiangyu Du,Jun Zhang,Liwei Liu,Zhuolun Li,Lianping Xue,Xin Liu,Zhi Sun
Purpose Shenkang injection, a traditional Chinese herbal prescription, had been widely used in renal disease due to its perfect curative effect. In this research, a novel, sensitive, accurate and rapid liquid chromatography-tandem mass spectrometric method was developed to simultaneously detect the seven active ingredients in rat plasma of Shenkang injection and investigate its pharmacokinetic behaviors with metabolism profiling meanwhile.Methods For accurate pharmacokinetic quantitation, a WATERS ACQUITY UPLC® BEH C18 column was used to perform a separation and acetonitrile-water (0.1% formic acid) was selected as mobile phase for gradient elution with a flow rate of 0.20 mL/min. A heated electrospray ionization with selective reaction monitoring mode was used to monitor the precursor-product ion transitions for all the analytes and IS.Results They all showed good linearity over a wide concentration range (r>0.996 3) and the lower limit of quantification (LLOQ) was 0.1–1.0 ng/mL for analytes. The validation parameters were all within the acceptable limits. Furthermore, for metabolism profiling study, metabolites of the seven ingredients were identified from the rat plasma based on the accurate mass and fragment ions. The metabolic pathways mainly focus on reduction, dehydration and conjugation.Conclusion This study provided an overview of disposition of Shenkang injection, which is highly instructive for better understanding the effectiveness and toxicity of this drug.
研究领域:
中药学
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药理学
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分析化学
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DOI
PubMed
高影响因子
FOOD CHEMISTRY
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2021
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IF 7.514
Wei Jia,Xixuan Wu,Rong Zhang,Lin Shi
As preservative are extensively applied to prevent the quality degradation of Hengshan goat meat sausages, safety assessment based on lipid and elucidation of dynamic change mechanism is urgently needed. The effect of preservatives on lipidome profiles of sausages was investigated using UHPLC-Q-Orbitrap. Totally, 9 subclasses of 70 characteristic lipids (Cer, DG, LPC, PC, PE, PI, PS, SM, TG) were quantified accurately (LOD with 0.68–2.96 μg kg −1 , LOQ with 2.25–9.79 μg kg −1 , RSD < 3%). The decrease of TG concentration was the most significant, from 1072.43 mg kg −1 in preservative-free samples to 838.53, 786.41 and 681.35 mg kg −1 in natamycin, potassium sorbate and sodium diacetate treated samples, respectively. With regard to preservation and nutrition, natamycin was a potential preservative than two other preservatives. Significant lipid variables were primarily associated with glycerophospholipid and sphingolipid metabolism. Integration of both techniques provided a guide for meat industries to control spoilage with innovative strategies.
研究领域:
食品科学
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营养学
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生物化学
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DOI
PubMed
高影响因子
ANALYTICAL LETTERS
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2024
·
IF 1.6
Zekun Tang,Huihui Wan,Huaishuan Zhang,Yu Zhang,Min Ju,Jinfeng Zhao,Yuming Sun,Lina Zhou,Qingxin Yin,Rui Cai,Qiang Xu,Yuming Song,Hua Zhang
As an important circulating metabolite in the body, the accurate determination of glucose in body fluids is very important for the evaluation of physiological status. However, liquid chromatography–mass spectrometry (LC–MS) methods present challenges for glucose due to poor ionization combined with weak chromatographic retention. Here, a method for determining salivary glucose using LC–MS after derivation by dibenzylamine is described in which 3-O-methyl-D-glucopyranose was used as internal standard. Saliva samples were prepared by protein precipitation, and the analytes were separated on a polar-copolymerized C18 reversed phase column. Detection took place by high-resolution orbitrap mass spectrometry after ionization in the positive mode. The calibration function was linear from 0.35 to 50 ng/mL. The recoveries were from 97.82 to 104.51% for intraday assays and 98.96 to 106.61% for interday assays. The intraday precision of salivary glucose was from 0.37% to 1.43% and the interday precision from 1.33% to 1.43%. The limits of detection and quantification in saliva were 0.2 and 0.6 ng/mL. The samples after derivatization were stored at 4 °C and 25 °C and analyzed every two days with five repeats. The relative standard deviations were 0.09% and 0.27% at 4 °C and 25 °C. This method was employed for the determination of the glucose in saliva for healthy male college students after exercise.
研究领域:
分析化学
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医学
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DOI
高影响因子
Arabian Journal of Chemistry
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2021
·
IF 5.165
Ruimin Wang,Ruiping He,Zhaohui Li,Xue Lin,Lu Wang
Rosa roxburghii Tratt. leaves (RRLs) have been exploited as a alternative tea product in China owing to its various biological properties. A comparative study was performed for the first time on high-performance liquid chromatography quadrupole orbitrap tandem mass spectrometry (HPLC-Q-Orbitrap-MS/MS) phenolic profiles, antioxidant, α -glucosidase inhibitory ( α -GIA) and anti-bacterial activities of the RRLs extracts extracted by traditional and eco-friendly solvents. The RRLs extracts extracted with four screened deep eutectic solvents (DES) showed higher total phenolic content (TPC, 167.48–190.14 mg GAE/g DW) and moderate total flavonoid content (TFC, 3.78–4.11 mg RE/g DW), while the RRLs extracts extracted with choline chloride-1,2-propanediol, choline chloride-levulinic acid, and 50% methanol/ethanol extracts had the highest TFC. Ethyl acetate extracts had the lowest TPC and TFC. Additionally, the phenolic constituents of the RRLs extracts were identified and quantified via HPLC-Q-Orbitrap-MS/MS and HPLC-DAD methods. A total of 30 phenolic compounds were identified in RRLs extracts. Among them, arbutin, gallic acid, (+)-catechin, 3-hydroxybenzoic acid, quercetin-3- O -galactoside and myricetin were the representative ones. The selected DES (especially for choline chloride-lactic acid and choline chloride-levulinic acid) extracts exhibited higher 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid (ABTS +• ) and 2,2-diphenyl-1-picrylhydrazyl (DPPH • ) scavenging activities, cupric reducing antioxidant capacity (CUPRAC), ferric reducing antioxidant power (FRAP) except for reducing power, α -GIA and anti-bacterial activity as compared with the extracts extracted with other solvents. Multivariate analysis results revealed that the extraction solvents significantly affected the phenolic constituents and biological activities of the RRLs extracts. The present study presented eco-friendly solvents for high-efficient extraction of the phenolic metabolites from RRLs. RRLs as a potential source enriched in phenolic constituents can be applied in the health, cosmetic and pharmaceutical industries.
研究领域:
植物化学
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食品科学
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药理学
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DOI
高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
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2023
·
IF 6
Zhenbao Jia,Hua Liu,Wenwei Chen,Fei Tao
Gynura bicolor DC ( G. bicolor ) is largely consumed as a vegetable in many parts of the world, and due to its content in anthocyanin can be considered as a health-promoting food. This study aimed to characterize the anthocyanin composition of G. bicolor and compare the effect of microwave vacuum drying (MVD) on the anthocyanin content with that of hot air drying (HAD). Anthocyanins were characterized using high-performance liquid chromatography-quadrupole-Orbitrap mass spectrometry (HPLC-Q-Orbitrap MS), which accurately identified five anthocyanin compounds. Delphinidin 3- O -neohesperidoside is the main anthocyanin compound found in G. bicolor . MVD decreased the drying time by 89% compared to HAD. MVD retained 87% of the total anthocyanins in G. bicolor , compared to 18% retained by HAD. This study revealed that MVD produced high-quality dried G. bicolor products, while exhibiting reduced processing times compared to those achieved using HAD.
研究领域:
食品科学
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植物化学
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产品关联
DOI
高影响因子
Journal of Analysis and Testing
·
2023
·
IF 4.7
Yang Jingxuan,Guo Wenjun,Xu Xiaohang,Zhao Liang,Xu Yajuan,Wang Yang
Fatty acids (FAs) are an important class of functional small molecules and participate in a variety of life biological processes. This experiment proposed a liquid chromatography–quadrupole-Qrbitrap mass spectrometry (LC–Q-Orbitrap MS) method to perform FA profiling under parallel reaction monitoring (PRM) acquisition mode. The FA was derivatized by 2-dimethylaminoethylamine (DMED) to increase the ionization efficiency and provide the characterized fragment pattern. The mass spectra obtained from full scan, multiple ion monitoring (MIM), and PRM were compared. The results showed that the protonated ion of FA + DMED–H 2 O was detected and the neutral loss of 45.06 Da was observed in the tandem mass spectrum. The PRM method provided the highest selectivity and sensitivity for FA detection with the help of accurate mass weight and specific neutral loss-based fragments. The method validation was performed using the FA standards and pooled quality control serum sample, which showed that the established method had good repeatability, stability, and linearity. Finally, the developed method was successfully applied to analyze the rat serum and brain tissue samples for the drug efficacy evaluation of gross saponin of Tribulus terrestris L. fruit (GSTTF) against middle cerebral artery occlusion (MCAO)-induced ischemic stroke. This method has extensive practicability and great potential in the detection of FA, especially for the analysis of samples with complex matrices.
研究领域:
分析化学
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药理学
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神经科学
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生物化学
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产品关联
DOI
高影响因子
Analytical Methods
·
2024
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IF 2.7
Jing Sun,Gao-Xu Xue,Xu Gong,Zai-Ping Zhang,Jie Xu,Lei Chen,Ling Cao,You-Long Feng,Yun-Jing Zhang
Chemical hair dye components can have allergenic, reproductive, and carcinogenic risks. Detecting restricted and prohibited ingredients in these products is challenging due to product diversity, isomer separation, instability, and wide polarity range. A method was developed using HPLC-high-resolution mass spectrometry for the qualitative and quantitative analysis of 54 hair dye components in various products. Samples were extracted with a 70% methanol solution, ultrasonicated in an ice bath, centrifuged, filtered, diluted with 25% methanol solution and 25% methanol solution containing 0.05% D-isoascorbic acid. Separation was achieved using an ACE Excel 3 C18 column (2.1 mm × 150 mm, 3 μm) with analysis conducted via quadrupole Orbitrap mass spectrometry. It showed good linear correlations, with detection limits of 0.1–23.5 ng mL−1, and quantitation limits of 0.2–78.1 ng mL−1. Average recovery ranged from 60.0% to 118.4%, with repeatability from 4.0% to 14.9%. Stability was confirmed within 48 hours. When applied to 20 batches of commercially available hair dyes, 24 hair dye components were found within permissible levels. The method is crucial for quality control of hair dyes, covering 10 common prohibited and 44 permissible hair dye components outlined in the Safety and Technical Standards for Cosmetics (2015 Edition). Compared to the standard methods, it can separate isomers in a single mobile phase system within 15 minutes in positive ion mode while maintaining sensitivity for phenol, hydroquinone, and other components in negative ion mode. Moreover, the pre-treatment strategy significantly improved stability and accuracy, enabling precise analysis of the 54 hair dye components.
研究领域:
分析化学
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药物分析
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毒理学
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化妆品科学
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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）