JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2023
·
IF 3.4
Jieping Zhao,Xiu Chen,Hengbin Zhang,Xiaoyan Liu,Yiwen Ma,Jianbiao Yao,Huidi Jiang,Hui Zhou
Shexiang Tongxin Dropping Pill (STDP) is a well-known compound preparation used in traditional Chinese medicine for treating cardiovascular diseases. Bufadienolides are the major active compounds of toad venom and are the key to the seven medicinal herbs that comprise STDP. In this study, a reliable and sensitive high-performance liquid chromatography-tandem mass spectrometry method was developed and validated for the quantitative determination of nine bufadienolides (bufalin, gamabufotalin, resibufogenin , marinobufagin , arenobufagin, desacetylcinobufagin, telocinobufagin, hellebrigenin, and hellebrigenol) in rat plasma and tissues (heart and liver). The chromatography column used was a Waters ACQUITY UPLC HSS-T3 column with gradient elution using mobile phase consisting of acetonitrile–water (0.1% formic acid added) at a flow rate of 0.25 mL/min. This method passed the methodological validation of plasma and tissues and was successfully applied to pharmacokinetic and tissue distribution studies after oral administration of STDP in healthy and ischemia-reperfusion (I/R) rats. This indicated that most bufadienolides were well absorbed and quickly distributed in the heart and liver. The area-under-the-curve (AUC) (0−t) of most analytes increased in a dose-dependent manner. Moreover, most of the tested components showed lower plasma and higher tissue concentrations in I/R rats than in healthy rats. The above results on the oral pharmacokinetics and tissue distribution may be helpful for the clinical application of STDP.
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高影响因子
Chinese Journal of Natural Medicines
·
2019
·
IF 1.773
Yan YAN,Qiang LI,Hui-Zhi DU,Chen-Xi SHEN,Ai-Ping LI,Xiang-Ping PEI,Chen-Hui DU,Xue-Mei QIN
ABSTRACT Ziziphi Spinosae Semen (ZSS) has been used for treatment of insomnia in China for centuries. To reveal the influence of insomnia on the levels of the neurotransmitters including serotonin (5-HT), glutamic acid (Glu), γ -aminobutyric acid (GABA), noradrenaline (NE) and dopamine (DA), and to study the role of ZSS aqueous extract in the treatment of insomnia, an UPLC-ESI- MS/MS method was developed and validated for simultaneous determination of five neurotransmitters in the rat brain. The brain samples were pretreated by one-step direct protein precipitation with acetonitrile. The analytes were detected in positive mode with multiple reaction monitoring (MRM) and the procedure was completed in less than 10 min. The method showed a good linearity ( R 2 > 0.9967) with the other validation parameters were within acceptance range. The results indicated that the concentration of 5-HT, GABA and DA is significantly lower ( P < 0.01) in para -chlorophenylalanine (PCPA)-induced insomnia rat model group, while Glu and NE significantly higher than those in control group ( P < 0.01). Treatment with ZSS aqueous extract (4 or 8 g·kg –1 ·d –1 for seven days) could ameliorate the symptoms of insomnia by significantly changing the levels of the neurotransmitter parameters mentioned above. The data obtained in this study demonstrate that ZSS aqueous extract could ameliorate the symptoms of insomnia by modulating the levels of monoamines and amino acid neurotransmitters in the brain.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2018
·Vol. 410
·期 25
·6619-6632
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IF 3.307
Li Shuo,Jia Mengtian,Guo Hongqiao,Hou Xiaohong
In this work, a variety of highly porous metal organic framework/chitosan (MOF/CS) foams (MIL-53(Al)/CS, MIL-53(Fe)/CS, MIL-101(Cr)/CS, MIL-101(Fe)/CS, UiO-66(Zr)/CS, and MIL-100(Fe)/CS) were designed and prepared by an ice-templating process. The introduction of MOFs made these foams achieve excellent inherent characters in terms of strength, stability, and adsorption ability. The MOFs incorporated in the foams retained their unique properties. Additionally, the foams were durable and their adsorption abilities had only a little loss after being recycled several times. MIL-53(Al)/CS foam was selected as an adsorbent candidate to develop an ultrasound-assisted solid-phase extraction (UA-SPE) method for the first time, owing to its particularly noteworthy performance among the prepared MOF/CS foams. The method was then successfully applied to extract trace amount of five parabens (methylparaben, ethylparaben, propylparaben, butylparaben, benzylparaben) in water samples, followed by ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) detection. Several experimental parameters were investigated. Under the optimal conditions, the linear ranges were 0.5–200 μg/L with regression coefficients ( r 2 ) from 0.9948 to 0.9983. The method detection limits were between 0.09 and 0.45 μg/L. The recoveries ranged from 78.75 to 102.1% with relative standard deviations (RSDs) < 7.4%. Furthermore, the molecular interactions and free binding energies between MOFs and parabens were calculated by means of molecular docking to explain the adsorption mechanism deeply. The novel method proposed in this work exhibited many benefits such as easy operation, high enrichment efficiency, less solvent consuming, and higher sensitivity. Such a strategy would expand the application prospect of MOFs in sample pretreatment.
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FOOD CHEMISTRY
·
2022
·
IF 9.231
Meng Wang,Jingjing Wang,Kangkang Wang,Liugen Zhang,Xianglei Cao,Cheng Guo,Jide Wang,Bin Wu
More and more attention has been paid to the improved QuEChERS (quick, easy, cheap, effective, rugged and safe) method in dealing complex sample matrices, especially for the study of QuEChERS adsorbents. In this study, a magnetic mesoporous material, which was derived from MIL-88B modified by l -alanine, was synthesized as modified QuEChERS adsorbents for the simultaneous determination of multiple pesticides (Methomyl, Isoprocarb, Carbofuran, 3-Hydroxycarbofuran, Acetamiprid, Imidacloprid) in Chinese cabbage, celery, long bean and leek. The prepared magnetic adsorbents can effectively remove interfering substances from the sample, and the proposed modified QuEChERS method can reduce sample pretreatment time via an external magnetic field. To achieve the best performance of QuEChERS method, the clean-up time and amount of QuEChERS adsorbents were investigated. Under the optimized conditions, a simple, rapid and sensitive method for the determination of 6 pesticide residues in vegetables was established by coupling the modified QuEChERS to ultrahigh-performance liquid chromatography-tandem mass spectrometry. Excellent sensitivity (The limit of detection for the 6 pesticides ranged from 0.001 to 0.020 µg kg −1 ), satisfactory linearity (r 2 ≥ 0.9952), good recovery (73.9–107.7%) and good precision (3.6–16.9% for intraday relative standard deviation, 0.5–15.0% for interday relative standard deviation) were obtained. Compared with traditional QuEChERS method, the proposed method is simple, cost-effective, and efficient, which indicates that the method can be used to detect carbamate and neonicotinoid pesticides in real samples and provide an excellent pretreatment technique for the detection of trace multi-analytes from complex substrates.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2022
·
IF 3.571
Yan Su,Lin Tao,Xiaoli Zhang,Xianjie Sheng,Qin Li,Wenying Fei,Tao Yin,An Kang,Jiye Aa,Guangji Wang
Dalitong Granules , a potent gastrointestinal motility promoting traditional Chinese medicine, is used to treat functional dyspepsia clinically. It shows good effect on alleviating gastrointestinal motility disorders and has a broad prospect of clinical application. However, there is no comprehensive study on its in vivo and in vitro chemical analysis. UPLC-Q-TOF-MS combined with the non-targeted characteristic filter analysis and in silico prediction strategies (NCFS) were used to deduce and identify the chemical components and in vivo metabolites in the bio-samples of rats following oral administration of Dalitong Granules . In this study, 108 chemical components were identified in Dalitong granules , including 50 flavonoids, 22 alkaloids, 13 terpenes, 11 organic acids, 10 coumarins and 2 volatile oils. In the plasma, tissue, urine and fecal samples of rats after administration of Dalitong granules , a total of 147 compounds were speculated (60 prototype compounds and 87 metabolites). The main metabolic pathways in vivo include methylation, demethylation, deglycosylation, hydrogenation, hydroxylation, sulfonation and glucuronidation as there are many flavonoids existing in Dalitong Granules . In conclusion, the chemical components and metabolites of Dalitong Granules were comprehensively identified by using a rapid and accurate analysis method, which laid a foundation for dissecting its bioactive substances. In addition, it provides a scientific basis for the in-depth study of the material basis of Dalitong Granules efficacy and its further comprehensive development and utilization.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2020
·Vol. 412
·期 8
·1807-1816
·
IF 3.637
Hu Xin,Liu Man,Liu Yifei,Zhang Jingjing,Tang Yuwen,Pei Hong,Liu Hegang,Chen Shilin,Song Chengwu,Hu Zhigang
Herbal materials have both medicinal and commercial values. As such, accurate species and content identification and verification are necessary to ensure the safe and effective use for medical and commodity purposes. Herein, we introduce a two-step approach for systematic identification and quality evaluation of wild and introduced Anemone flaccida Fr. Schmidt (aka Di Wu) using DNA barcode and ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS/MS). To begin, a precise and rapid identification method based on internal transcribed spacer 2 (ITS2) sequence was developed to ensure the authenticity of ‘Di Wu’ species. Next, the major active components were fully characterized utilizing a targeted profile of oleanane-type triterpenoid saponins, which was established via UPLC-QTOF-MS/MS. As a result, 34 oleanane-type triterpenoid saponins were identified or characterized in ‘Di Wu.’ The qualitative and relative quantitative analysis showed obvious differences between wild and introduced ‘Di Wu.’ Furthermore, dynamic changes in the contents of triterpenoid saponins throughout various harvesting periods were clearly explained and mid-April was identified as the appropriate harvest time. Moreover, results indicate that the contents of five main saponins (anhuienoside E, glycosideSt-I4a, hemsgiganoside B, flaccidoside II, and hederasaponin B) are more appropriate as a quality evaluation indicator than the current quality standard. The two-step approach provides a suitable strategy to evaluate the genuine quality of wild and introduced ‘Di Wu,’ and can be applied to the targeted analysis of other triterpenoid saponin analogues for quality evaluation.
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FITOTERAPIA
·
2025
·
IF 2.6
Wenjing Ren,Yue Zhou,Jiahui Zhao,Xiutong Ge,Shiru Jiang,Yang Chen,Gui Xu,Shuo Zhang,Li Li,Ji Shi,Fan Zhang
Songaria Cynomorium Herb (SCH), a traditional Chinese medicinal herb, is recognized for its dual role as both a dietary supplement and a therapeutic agent. It is traditionally reputed to have kidney-tonifying and Yang-strengthening effects, which have made it a common ingredient in nutritious food supplements and health products. This study investigates the underlying mechanisms by which wine-steamed SCH, enhances kidney aphrodisiac qualities, focusing on the tyrosine kinase/signal transduction and transcriptional activation factor (JAK/STAT) signaling pathway. Ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) was employed to qualitatively analyze the chemical constituents of SCH both before and after the wine-steaming process, and the significant differential components were screened out. A kidney-Yang deficiency model was induced by intragastric administration of hydrocortisone. Subsequently, the rats were treated with either raw SCH (RSCH) or wine-steamed SCH (WSCH) medicinal solutions. Urine output, organ indices, target gland axis-related indices, and renal tissue lesions were recorded and statistically compared between the treatment and control groups. RT-qPCR and Western blot analysis were utilized to assess the mRNA and protein expression levels of the JAK/STAT pathway and HIF-1α in the renal tissues of the animals. The results indicated that the chemical composition of the SCH underwent changes before and after the steaming process. The tonifying effects observed were more pronounced with WSCH than with RSCH, suggesting that the mechanism involves the inhibition of the JAK/STAT pathway and the downregulation of HIF-1α expression.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2026
·
IF 3.4
XiangLong Chen,Jinhui Xu,Chengliang Wang,Lijuan Yang,Jinwei Fan,Tongtong Li,Qian Zhang,Yanxia Yu,Lian Tang,Shenjia Huang
Central nervous system (CNS) infections require adequate drug exposure at the site of action, yet antibiotic meropenem (MER) shows limited cerebrospinal fluid (CSF) penetration and easily undergoes non-enzymatic degradation to an inactive open-ring metabolite (ORM). In this study, we developed a simple, sensitive, and fast liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the simultaneous determination of MER and ORM in human serum and CSF. Chromatographic separation was accomplished on an Agela Venusil MP C18 column, with MER-d6 and ORM-d6 as internal standards. Methanol was found to promote methanolysis, yielding a characteristic product ( m/z 416.2). Therefore, acetonitrile was selected as both the organic phase and the protein-precipitation solvent. Method validation was conducted according to the ICH M10 guideline. Follow validation, the method was successfully applied to 57 serum and 16 CSF samples. ORM concentrations in human CSF were reported for the first time. This method provides a valuable tool to support MER monitoring in patients with CNS infections.
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BIOMEDICAL CHROMATOGRAPHY
·
2021
·Vol. 35
·期 10
·e5174
·
IF 1.902
Yuan Lu,Na Li,Xiaoqin Zhu,Jie Pan,Yonglin Wang,Yanyu Lan,Yongjun Li,Aimin Wang,Jia Sun,Chunhua Liu
Polygonum orientale L . is a traditional Chinese medicine having extensive pharmacological activities including antimyocardial ischemia (MI) injury properties. Isoorientin, orientin, vitexin, quercitrin, astragalin and protocatechuic acid are the main compounds in P. orientale extract. The aim of this study was to establish an ultra-performance liquid chromatography–tandem mass spectrometry method for the determination of the content of these compounds in urine, feces and bile samples simultaneously and application of the method in a comparative excretion study in normal and MI model rats after oral administration of P. orientale extract. Chromatographic seperation was conducted on an Agilent Eclipse Plus C 18 column with the mobile phase consisting of 0.1% formic acid–acetonitrile and 0.1% formic acid–water. Negative ion multiple reaction monitoring mode was used for quantification. The six compounds had good linearity ( r ≥ 0.9921) and acceptable accuracy ranging from 10.10 to −5.82% The relative standard deviations of within-day precision and inter-day precision were <10.45 and 13.44%, respectively. The extraction recovery of the six analytes ranged from 80.31 to 101.47% and the matrix effect was 82.56–102.88%, indicating that the preparations of sample collected form urine, feces and bile were stable throughout analysis. The excretion amount of the six analytes increased in both normal and MI model rats’ urine, feces and bile in a 24 h period and became stable between 36 and 48 h after administration. The total excretion rate of six compounds was <5% in urine, feces and bile of normal and MI model rats. The excretion peak period for all compounds in MI rats was slower than that in normal rats. This excretion study provides insights for further application and research on P. orientale .
研究领域:
药理学
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分析化学
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中药学
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ANALYTICAL LETTERS
·
2023
·
IF 2
Zheqi Fei,Baisen Chen,Xuemei Wei,Lili Lian,Xiyue Wang,Dawei Lou
Developing highly efficient adsorbents toward trace pollutant analysis in complex biological samples is a challenge in analytical chemistry. Herein, NiO/ZnO-coated carbon microspheres (denoted by NiO/ZnO@C) with a well-defined core–shell structure were prepared through hydrothermal treatment and subsequent pyrolysis in air to enrich malachite green (MG) and crystal violet (CV). Hydrophilic carbon microspheres played an important role in the formation of core–shell NiO/ZnO@C, which may lead to the deposition of Ni2+/Zn2+ upon the surface via acidic chelating ligands. Based on the Langmuir model, NiO/ZnO@C demonstrated high adsorption capacities of 333.3 and 192.3 mg/g for MG and CV, respectively. Moreover, the NiO/ZnO@C composite served as a dispersive solid-phase extraction adsorbent to determine MG and CV in aquatic products combined with ultra-high performance liquid chromatography. High linearity was obtained for analyte concentrations from 5 to 500 μg/L with correlation coefficients (r) exceeding 0.9991. The limits of detection of the method were 0.50 μg/L (MG) and 0.35 μg/L (CV) with relative standard deviations less than 7.47%. Furthermore, the developed method was employed to determine MG and CV in aquatic products.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2016
·
IF 2.687
R. Xu,H.T. Gao,F. Zhu,W.X. Cao,Y.H.M. Yan,X. Zhou,Q. Xu,W.L. Ji
This research was mainly focused on the effects of food emulsifier on the bioavailability of six priority controlling phthalate acid esters (PAEs) for the further accurate assessment of their toxic effects, using the corresponding phthalate acid monoesters (PAMEs) in rats urine as biomarkers. Glycerin monostearate was chosen as typical food emulsifier. A method was established to determine PAMEs in urine from rats either in experimental group (integrated gavaged with glycerin monostearate and PAEs) or in control group (gavaged with PAEs only), by using solid-phase extraction (SPE) coupled with ultra performance liquid chromatography tandem mass spectrometry (SPE–UPLC–MS/MS). Extraction recoveries were more than 75% for all the PAMEs; the calibration curve was linear in the range of 1.0–1000.0 ng/mL with R 2 > 0.995; the limits of detection (LOD) were 0.30 ng/mL–0.50 ng/mL. In addition, by analysing quality control (QC) urine samples in 3 days, it showed that the method was precise and accurate, for the intra-day and inter-day RSD within 16%, and the accuracy more than 82%. Internal exposure amount of all PAEs in experimental group was significantly higher than that in control group with p values of less than 0.05 except for butyl benzyl phthalates (BBP) ( P = 0.07). The bioavailability of all PAEs ranged from 5.03% to 109.35% with the presence of food emulsifiers glycerin monostearate, observably higher than that without glycerin monostearate (1.12% to 54.39%). It indicated that food emulsifiers increased the bioavailability of PAEs and may lead to potential food safety risk, which should bring awareness and be further studied.
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FOOD CHEMISTRY
·
2025
·
IF 9.8
Yiheng Li,Xue Yang,Qimin Zhang,Longlin Wang,Huiyuan Guo,Xuhui Chen,Yantao Guo,Xiuping Li,Weibing Zhang,Pengjie Wang,Pengcheng Wen
Zhaiji millet vinegar (ZJMV) is a traditional grain-fermented condiment whose quality improvement is associated with aging time. This study revealed the evolution of physicochemical properties and whole-component of ZJMVs aging 2 to 10 years. Results demonstrated pH, chroma, and the content of total acid, reducing sugar, and amino acid nitrogen fluctuate dynamically, while antioxidant activities were significantly correlated with the content of total flavonoids, total phenols, tetramethylpyrazine, amino acids, and organic acids ( p < 0.05). GC-IMS and metabolomics identified 47 volatile organic compounds (VOCs) and 6530 metabolites, with 6 differential VOCs and 19 differential metabolites ( p < 0.05, variable importance in projection (VIP) > 1, fold change (FC) < 0.5 or > 2) being shared aging markers. KEGG pathway analysis indicated amino acid metabolism enriched the most differential metabolites, whereas biosynthesis of various alkaloids was critical. Our findings provide novel mechanistic insights into the quality development of ZJMV during aging.
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