RSC Advances
·
2018
·Vol. 8
·期 5
·2459-2468
·
IF 2.936
Dan Zhang,Yun-ling Gao,Sheng Jiang,Yiwen Chen,Yi Zhang,Zheng Pan
Lamiophlomis rotata (L. rotata) is a Tibetan medicinal herb used for centuries that contains iridoid glycosides (IGs), which are pharmacologically active ingredients and can be used for quality control. The IG profiles of the underground and aerial parts of the plant were determined by UPLC-TOF-MS to evaluate the similarity and variability of the different herbal parts listed in the Chinese Pharmacopoeia. Twenty-six IGs were detected in the total ion current (TIC) profile of L. rotata, and twenty-two of these were identified by comparing the retention times and mass spectra of the compounds to those of authentic standards. Among these compounds, five IGs with the same molecular formula (C17H26O11) were identified for the first time by mass spectrometry based on their different hydroxyl group-substituted positions. The aerial part has a similar chemical profile to that of the roots. The difference between the two parts was determined by multivariate statistical analysis of the UPLC-TOF-MS data of 24 specimens. Sesamoside was explored as the most characteristic marker to distinguish the two parts of L. rotata. To further estimate the distinction between the two parts, the content of total IGs and the antioxidant capacity were investigated in samples from different locations. The aerial parts showed a high content of total IGs and high antioxidant capacity, although not higher than those of the roots. The results also suggest the dosage should be increased when the aerial parts are used as crude medicinal materials instead of the underground parts.
研究领域:
药用植物学
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中药化学
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质量控制
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Yingxia Guo,Jiaxin Zhang,Runran Mei,Zihan Tang,Meichen Liu,Xixian Weng,Meiyun Shi,Lei Yin
Addressing critical gaps in understanding the in vivo behavior of polyethylene glycol (PEG)-based excipients, this study systematically elucidates the biological fate of methoxy-PEG₆-hydroxyl (M-PEG₆-OH) through comprehensive pharmacokinetic and metabolic investigations in rats. Employing a validated ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) methodology, we reveal distinctive biodistribution characteristics including rapid systemic clearance (Half-life (t 1/2 ) = 1.92 ± 1.16 h) and extensive tissue penetration (Apparent volume of distribution (V d ) = 0.84 ± 0.45 L/kg), suggesting efficient extravascular dissemination. Excretion pathways analysis demonstrated predominant renal elimination, with 59.03 % of the administered dose recovered in urine within 48 h post-IV injection, contrasting with minimal fecal excretion (0.99 %). Quantitative metabolite profiling identified M-PEG₅-CH₂COOH as the oxidative transformation product through terminal hydroxyl modification. The significantly higher relative abundance of metabolites (M-PEG 5 -CH 2 COOH) in urine compared to feces within the same time period provides critical insights into the biotransformation processes and metabolic pathways of the PEG polymer. These findings establish the first systematic evidence of metabolic trajectory and elimination mechanisms for M-PEG-OH, offering vital references for optimizing PEGylated drug delivery systems with enhanced biocompatibility and predictable safety profiles.
研究领域:
药代动力学
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分析化学
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生物化学
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药剂学
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代谢
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DOI
PubMed
高影响因子
ULTRASONICS SONOCHEMISTRY
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2025
·
IF 9.7
Hongke Wei,Xiaomin Wang,Jiaqi Wang,Shijie Ren,Luis A.J. Mur,Dong Lu,Duo Cao
To valorize sour jujube ( Ziziphus acidojujuba ) leaves, this work focused on the extraction, quantification, and bioactivity assessment of flavonoids. First, ultrasound-assisted extraction (UAE) was employed to extract total flavonoids from sour jujube leaves (SJL-TF), with the procedure optimized through single-factor design and response surface methodology (RSM). SJL-TF yield reached 48.47 ± 0.36 mg/g under optimal circumstances, which included 61 % ethanol as extraction medium, an ultrasound power of 300 W, an extraction time of 33 min, and a liquid–solid ratio of 16 mL/g, showing higher extraction efficiency in comparison to the traditional Soxhlet extraction method. Scanning electron microscopy (SEM) analysis indicated that ultrasound treatment severely damaged the structural integrity of sour jujube leaves, which was more conducive to improving the SJL-TF yield. Then, polyamide resin chromatography was used to purify the crude SJL-TF extracts, increasing the SJL-TF purity by 3.2-fold to 74.58 ± 0.63 %. By developing and validating a UPLC-QQQ-MS/MS method, ten main flavonoids in SJL-TF extracts, including catechin, rutin, isoquercetin, narirutin, nicotiflorin, quercitrin, phlorizin, luteolin, quercetin, and apigenin, were successfully detected concurrently for quality control purposes. Furthermore, the purified SJL-TF showed a strong ameliorative effect on dextran sulfate sodium (DSS)-induced ulcerative colitis (UC) in mice, as evidenced by significant mitigation of colonic inflammation and pathological damage. Thus, this work will contribute to improving the application of sour jujube leaves, especially in the pharmaceutical sector.
研究领域:
药理学
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分析化学
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植物化学
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DOI
PubMed
高影响因子
Analytical Methods
·
2016
·Vol. 8
·期 17
·3550-3563
·
IF 1.915
Man-Yun Chen,Yong-Jun Tang,Yi-Cheng Wang,Chong-Zhi Wang,Chun-Su Yuan,Yao Chen,Zhi-Rong Tan,Wei-Hua Huang,Hong-Hao Zhou
The compound medicine of betamethasone sodium phosphate (BSP) and betamethasone dipropionate (BDP) is widely used for the treatment of diverse glucocorticoid-sensitive acute and chronic diseases such as asthma, rheumatoid arthritis and systemic lupus erythematosus. It will be useful and beneficial to validate a sensitive method for the determination of BSP, BDP and their metabolites for a pharmacokinetic study. Hereby, ultra-high pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been validated for the determination of BSP, BDP and their metabolites betamethasone (BOH), betamethasone 17-monodipropionate (B17P) and betamethasone 21-monodipropionate (B21P) in human plasma. Liquid–liquid extraction with ether and n-hexane (v/v, 4 : 1) was used for sample preparation of BDP, BOH, B17P and B21P with beclomethasone dipropionate as the internal standard (IS), while solid phase extraction was adopted for sample preparation of BSP using prednisolone as the IS. Chromatographic separation was performed on a Hypurity C18 column (150 mm × 2.1 mm, 5 μm) for BOH, BDP, B21P and B17P, and a Luna C18 (2) column (150 mm × 2.0 mm, 5 μm) for BSP. Electrospray ionization interfaced with positive multiple reaction monitoring (MRM) scan mode was used for mass spectrometric detection. The standard calibration curves were linear within the range of 2.525 × 10−9 to 403.9 × 10−9 mol dm−3 for BSP, 0.125 × 10−9 to 55.81 × 10−9 mol dm−3 for BDP, 0.278 × 10−9 to 74.95 × 10−9 mol dm−3 for BOH, 0.098 × 10−9 to 4.688 × 10−9 mol dm−3 for B17P and 0.226 × 10−9 to 5.411 × 10−9 mol dm−3 for B21P, respectively. The validated method was successfully applied to a bioequivalence study in 23 healthy subjects after they were injected with this compound medicine BSP and BDP.
研究领域:
药物分析
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临床药理学
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DOI
PubMed
高影响因子
Current Pharmaceutical Analysis
·
2023
·Vol. 19
·期 6
·511-520
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IF 0.6
Zhang Mengmeng,Zou Qiaogen
Background: Atopic dermatitis (AD) is an allergic skin disease that can be inherited. Crisaborole is a specific drug developed to deal with this disease. The compounds of 4-(4- Bromo-3-formyl-phenoxy)-benzonitrile and 4-(4-(4-bromo-3-formylphenoxy)-3- formylphenoxy) benzonitrile
are the representative impurities in the synthesis of Crisaborole active pharmaceutical in gradient (API). Owing to the genotoxic impurities that could lead to cancer and gene mutations, it is necessary to develop a simple, efficient, sensitive, and accurate method to detect these impurities.
In this study, the 4-(4-Bromo-3-formyl-phenoxy)-benzonitrile and 4-(4-(4- bromo-3-formylphenoxy)-3-formylphenoxy)benzo- nitrile present in Crisaborole API were detected using UPLC-MS/MS. Methods: The separation was made on a ZORBAX Eclipse XDB-Pheny column (4.6 mm ×75mm, 3.5
μm) with the mobile phase of acetonitrile solution containing 0.1% trifluoroacetic acid (A) and water containing 0.1% formic acid (B) in gradient elution mode. Quantification was performed using positive ion electrospray ionization (ESI), and the contents of two compounds were determined
using the multiple reaction monitoring (MRM) modes. Results: The quantitative analytical method was fully validated with respect to linearity (r > 0.9998), sensitivity, precision, accuracy (the average recovery of two impurities was 84.1% to 90.7%), and robustness. Conclusion:
Three batches of samples were detected by UPLC-MS/MS, indicating that the proposed approach was applicable for the quality evaluation of Crisaborole.
研究领域:
药物分析
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皮肤病学
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毒理学
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DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2021
·
IF 3.935
Yujiao Zhao,Shanshan Chu,Shuangying Gui,Yuejian Qin,Rui Xu,Tingyu Shan,Huasheng Peng
Heshouwu , derived from root tubers of Fallopia multiflor a (Thunb.) Harald., is a well-known herb used for millennia in traditional Chinese medicine. However, different forms of root tubers of Heshouwu have occurred in current Chinese herbal market and used in clinic, although it is still unknown whether their quality is consistent. In the present study, a mass spectrometry imaging and laser microdissection combined with UPLC-Q/TOF-MS were therefore used for the metabolite profiling on the whole and different parts of root tubers of F. multiflora and F. multiflora var. angulata . Our results suggested that the character of “woody heart” root tubers of F. multiflora was similar to that of F. multiflora var. angulata , but the latter had more phloem fibers and larger diameter vessel in the normal vascular bundle. Moreover, 140 compounds including stilbenes, anthraquinones, phenolic acids, naphthalenes, and other compounds were identified or putatively characterized from F. multiflora and F. multiflora var. angulata . Both unsupervised principal component analysis (PCA) and supervised Orthogonal Partial Least Squares Discrimination Analysis (OPLS-DA) multivariate statistics allowed discriminating F. multiflora and F. multiflora var. angulata . And a total of 32 potential markers were identified. The tissue-specific study indicated that the compounds in the phelloderm of F. multiflora and F. multiflora var. angulata were the most abundant. This is the first study on metabolite profiling and comparison of root tubers between F. multiflora and F. multiflora var. angulata , which would provide reasonable basis for further quality evaluation and safe medication of F. multiflora .
研究领域:
中药学
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植物代谢组学
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产品关联
DOI
PubMed
高影响因子
Legal Medicine
·
2023
·
IF 1.5
Shan Zhang,Shunqin Chen,Faze Zhu,Aimin Wang,Bing Xia,Jie Wang,Jiang Huang,Yubo Liu,Peng Luo
Toxic alkaloids are typically found in herbal medicines and have strong pharmacological effects and a broad therapeutic spectrum. On the other hand, toxic alkaloids exert toxicological activities in vivo ; as such they have a narrow therapeutic window and can induce poisoning due to incorrect dose or misuse. In this view, there is an urgent need to develop a rapid and sensitive assay to detect these toxic alkaloids. This study developed a method for determining five common toxic alkaloids in blood, including brucine, strychnine, aconitine, mesaconitine, and hypaconitine using ultra-high liquid chromatography-tandem quadrupole/linear ion trap mass spectrometry (QTRAP UPLC–MS/MS). The analytes in this investigation were extracted with ether and detected using multiple reaction monitoring (MRM)-information-dependent acquisition (IDA)-enhanced product ion (EPI) scanning modes. SKF 525A served as the internal standard (IS). The approach demonstrated excellent linearity, with a correlation coefficient (R) > 0.9964, and satisfactory sensitivity, with the limit of detection (LOD) of 0.31 ∼ 3.26 ng/mL and a limit of quantification (LOQ) of 1.13 ∼ 11.52 ng/mL. The extraction recovery (ER) was 78.8 ∼ 116.2%, the matrix effect (ME) was −12.3 ∼ 21.2%, and the method accuracy was 0.8 ∼ 12.8%. In addition, the intra-day precision and the inter-day precision (RSD) were 0.7% ∼ 7.4% and 0.4% ∼ 13.5%, respectively. The developed approach is sensitive and efficient, and offer significant application prospect in clinical monitoring and forensic detection of poisoning.
研究领域:
分析化学
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法医学
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临床毒理学
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2024
·
IF 3.8
Huo Jinfeng,Zhe Wei,Zhang Yipeng,Yang Qianxu,Zeng Zhongda
The chemical components of natural fragrant plant extracts are of high complexity, and the strategies for quality control (QC) and further discovery of fragrance mechanisms still need to be further investigated. This study integrated the strategies and methods of untargeted metabolomics and chemometrics and statistical modeling to attain the goal. The techniques of reversed-phase and HILIC analysis of ultra-performance liquid chromatography-high-resolution mass spectrometry (UPLC-HRMS) were simultaneously used to collect data in both positive and negative ion modes. The pattern analysis of fingerprints and discovery of characteristic molecular markers for QC analysis were comprehensively employed to reach in-depth analysis of the quality variation and discovery of differential molecules among natural fragrant plant extracts. The former uses fingerprint technique to analyze their overall similarities and differences, and the latter comprehensively discovers molecular substances characterizing the chemical characteristics of fragrant extracts with the help of metabolomics and univariate and multivariate methods. The findings are expected to be used as the molecular markers in product manufacturing, sales, and consumption to achieve accurate quality control and recognition of targeted molecules for potential quality monitoring using spectroscopy techniques. In this work, 27 natural fragrant extracts were applied as examples, and their chemical components were comprehensively analyzed with discovery of markers for quality control. After data integration, 1178 molecules were annotated, and 267 differential metabolite molecules with the values of variable importance in the projection (VIP) larger than 1.0 were found. The results show that the method proposed in this work is of great significance for high-coverage analysis, QC marker discovery, and aroma mechanism elucidation, which has potential applications in the areas of food, cosmetics, pharmaceuticals, tobacco, and others. Graphical Abstract
研究领域:
分析化学
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植物学
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食品科学
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药学
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产品关联
DOI
PubMed
高影响因子
INTERNATIONAL JOURNAL OF FOOD SCIENCE AND TECHNOLOGY
·
2017
·Vol. 52
·期 4
·897-905
·
IF 1.64
Fangfang Zeng,Zhiwei Ge,Jarukitt Limwachiranon,Li Li,Simin Feng,Yansheng Wang,Zisheng Luo
Summary The content of bioactive phytochemicals, antioxidant activity and tyrosinase inhibitory activity of the hydroalcoholic extracts of Rosa roxburghii were determined. Yellow fruits of cultivated R. roxburghii showed the highest phenolic content (154.81 mg gallic acid g −1 ), and the green fruits of wild R. roxburghii showed higher content of flavonoid and triterpenoid. Rosa roxburghii fruits from different cultivars and maturity stages all demonstrated as good antioxidant agents and tyrosinase inhibitors, with IC50 value about twice of the positive standard in the DPPH assay and triple of the standard in the tyrosinase inhibitory activity assay. Nineteen compounds, mainly ellagic acids and its derivatives, flavonoids and their glycosides were identified by UPLC-Triple-TOF/MS analysis. As the first study of bioactive phytochemicals of R. roxburghii by UPLC-MS, the present research may provide valuable information for fulfilling the potential of R. roxburghii in the functional food area.
研究领域:
植物学
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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
CHEMICO-BIOLOGICAL INTERACTIONS
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2016
·
IF 2.618
Xia Wu,Jian-Cheng Zhu,Yu Zhang,Wei-Min Li,Xiang-Lu Rong,Yi-Fan Feng
Potential impact of lipid research has been increasingly realized both in disease treatment and prevention. An effective metabolomics approach based on ultra-performance liquid chromatography/quadrupole-time-of-flight mass spectrometry (UPLC/Q-TOF-MS) along with multivariate statistic analysis has been applied for investigating the dynamic change of plasma phospholipids compositions in early type 2 diabetic rats after the treatment of an ancient prescription of Chinese Medicine Huang-Qi-San. The exported UPLC/Q-TOF-MS data of plasma samples were subjected to SIMCA-P and processed by bioMark, mixOmics, Rcomdr packages with R software. A clear score plots of plasma sample groups, including normal control group (NC), model group (MC), positive medicine control group (Flu) and Huang-Qi-San group (HQS), were achieved by principal-components analysis (PCA), partial least-squares discriminant analysis (PLS-DA) and orthogonal partial least-squares discriminant analysis (OPLS-DA). Biomarkers were screened out using student T test, principal component regression (PCR), partial least-squares regression (PLS) and important variable method (variable influence on projection, VIP). Structures of metabolites were identified and metabolic pathways were deduced by correlation coefficient. The relationship between compounds was explained by the correlation coefficient diagram, and the metabolic differences between similar compounds were illustrated. Based on KEGG database, the biological significances of identified biomarkers were described. The correlation coefficient was firstly applied to identify the structure and deduce the metabolic pathways of phospholipids metabolites, and the study provided a new methodological cue for further understanding the molecular mechanisms of metabolites in the process of regulating Huang-Qi-San for treating early type 2 diabetes.
研究领域:
代谢组学
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中医药学
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生物信息学
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DOI
高影响因子
MICROCHEMICAL JOURNAL
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2024
·
IF 4.9
Yan Qiao,Menglin Wang,Erling Guo,Ke Wang,Ling Ma,Kaoqi Lian
This study aimed to design and synthesize a novel adsorbent Fe 3 O 4 @SiO 2 @MPA-TAPA-COF material for the first time and used as an adsorbent of MSPE. It had significant potential for the pretreatment of trace analytes. The MSPE was coupled with ultra performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) for the rapid extraction and detection of 12 sulfonamides (SAs) from water and milk samples for the first time. Several experimental parameters were optimized, including adsorbent dosage and the effects of pH, ionic strength, adsorption time, and desorption conditions. Under the optimized pretreatment and instrumental conditions, good linearity of 0.1–100 μg·L −1 with a correlation coefficient 0.9994–0.9999, low limits of detection (0.004–0.044 μg·L −1 ) and limits of quantitation (0.013–0.136 μg·L −1 ) were obtained. Moreover, the recoveries of sulfonamides in water and milk samples were in the range of 60.88 %-102.94 %, and the relative standard deviations not exceeding 9.62 %. Finally, the magnetic Fe 3 O 4 @SiO 2 @MPA-TAPA-COF material possessed the magnetic separation and high adsorption affinity for extracting SAs from real samples. This study holds great significance in enhancing the monitoring of SAs drug residues in water and milk.
研究领域:
分析化学
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环境科学
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食品科学
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产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2017
·
IF 3.255
Xiaoxue Liu,Chenrong Huang,Ling Xue,Qingqing Xu,Wen Xia,Xing Li,Liyan Miao
A rapid and highly sensitive liquid chromatography-tandem mass spectrometry (LC–MS/MS) method has been developed and validated for the determination of a novel anti-HBV compound Y101 and its metabolites M8 and M9 in human plasma. The plasma samples were deproteinated with acetonitrile after addition of Peramivir (internal standard, IS) and separated on a 40 °C ACQUITY UPLC BEH C 18 column (2.1 mm × 50 mm, 1.7 μm). The mobile phase consisted of water (containing 5 mM ammonium acetate and 0.1% formic acid) and acetonitrile (74:26, v/v) at a flow rate of 0.3 mL/min. The detection was performed on a Triple Quad 5500 tandem mass spectrometer coupled with electrospray ionization (ESI) source in positive mode. Quantification was conducted by multiple reaction monitoring (MRM) of the transitions of m / z 490.1 → 339.0 for Y101, m / z 357.2 → 105.2 for metabolite M8, m / z 373.1 → 105.1 for metabolite M9 and m / z 329.1 → 270.2 for IS, respectively. The method was validated over the calibration curve range of 1.000–1000 ng/mL for Y101, 2.000–2000 ng/mL for metabolite M8 and 0.3000–300.0 ng/mL for metabolite M9, using linear regression and 1/x 2 weighting. No matrix effect and carryover effect was observed. The intra- and inter-batch precision and accuracy of Y101, metabolite M8 and M9 were all within the acceptable criteria. This method allows a rapid and simple determination of Y101 and its metabolites M8 and M9 in human plasma. It was successfully applied in a pharmacokinetic study in human for the first time.
研究领域:
药理学
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分析化学
·
临床药理学
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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）