BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 6
·e70108
·
IF 1.7
Ancheng Gu,Chuwen Zhang,Dan Li,Bohong Cen,Wanwen Cao,Zhongyuan Xu
Dapagliflozin is a widely used sodium-glucose cotransporter 2 inhibitor that has been approved for the treatment of Type 2 diabetes. In this study, we present a simple and sensitive high-performance liquid chromatography tandem mass spectrometry (HPLC–MS/MS) method for the simultaneous quantification of dapagliflozin and its metabolite, dapagliflozin 3-O-glucuronide (D3OG). The experiments were conducted using an Agilent G6495B triple quadrupole mass spectrometer coupled with an Agilent 1290 Infinity II HPLC system, featuring a Poroshell 120 EC-C18 column. Gradient elution was performed with ammonium formate (10 mM) and methanol as the mobile phase. The G6495B was operated in negative ion mode with electrospray ionization and multiple reaction monitoring. The quantitative method was validated according to FDA and EMA guidelines, assessing parameters such as selectivity, linearity, accuracy, precision, dilution integrity, stability, and recovery. Methanol was used as a protein precipitant during sample preparation, resulting in consistent extraction recoveries ranging from 91% to 96% for all analytes. The linear range for the analytes was established at 2–800 μg/L with a sample volume of 100 μL. This validated method is sufficient for the simultaneous quantification of dapagliflozin and D3OG in plasma and has been successfully applied in pharmacokinetic studies, bioequivalence assessments, and clinical therapeutic monitoring. Trial Registration: Chinese Clinical Trial identifier: ChiCTR2100044600
研究领域:
分析化学
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药理学
·
临床医学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 4
·e70038
·
IF 1.7
Mengjiao Li,Fuqiang Liu,Lulu Guo,Wu Fan,Jiazhong Wang,Binbin Lu,Guangfeng Hong,Wenjuan Zhang,Shu Tian,Jian Mao,Jianping Xie
Cordycepin, a natural adenosine derivative, exhibits multiple pharmacological effects on organisms. However, its distribution and metabolic characteristics have not been fully elucidated in vivo. In this study, ultra-high liquid chromatography tandem high-resolution mass spectrometry (UHPLC-HRMS/MS) was used to investigate the pharmacokinetic characteristics and effects of cordycepin on endogenous adenosine and inosine. Microdialysis was used for real-time monitoring of unbound drug in brain and blood, whereas conventional tissue homogenate methods assessed distribution in various tissues. Results showed that the distribution pattern of cordycepin was as follows: kidney > liver > heart > lung > spleen > brain. Cordycepin administration significantly altered the levels of adenosine and inosine in heart and liver. Synchronous microdialysis sampling for the pharmacokinetic profile indicated that cordycepin was rapidly consumed and 3′-deoxyinosine was generated as the main metabolite. The C max values of cordycepin in the rat blood and brain after exposure (10 mg/kg, i.p.) were 7.8 and 5.4 ng/mL, respectively. Mean residence time in blood and brain was 102.2 and 137.0 min, respectively. Inhibition of adenosine deaminase by racemic 9-(2-hydroxy-3-nonyl) adenine hydrochloride (EHNA) enhanced cordycepin levels in the blood. This work provides a solid basis for understanding the metabolism of cordycepin and its pharmacological effects.
研究领域:
药理学
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分析化学
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生物化学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 5
·e70083
·
IF 1.7
Yonghua Hu,Xujin Yang,Chenmei Ma,Zhen Wang,Xin Yuan,Man He,Penghai Zhang,Yi Tao
Da-Huang-Zhe-Chong Pills (DHZCPs) have demonstrated efficacy in treating uterine fibroids (UFs), but the mechanisms underlying their action remain unclear. In this study, untargeted serum metabolomic analysis was employed to investigate the therapeutic effects of DHZCP in a rat model of UFs utilizing advanced ultra-performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS) and pattern recognition. Histopathological examination through H&E staining revealed significant improvements in uterine morphology following DHZCP administration. The levels of four serum hormones, that is, estradiol (E 2 ), follicle-stimulating hormone (FSH), luteinizing hormone (LH), and progesterone (PROG), tended to shift toward normal in the DHZCP-treated group compared with the model group. Our metabolomic profiling identified 20 distinct endogenous metabolites that were differentially expressed between UF and normal rats, with DHZCP treatment significantly normalizing 16 of these metabolic markers. Comprehensive pathway analysis highlighted three major metabolic pathways affected by DHZCP intervention: tryptophan metabolism, riboflavin metabolism, and arginine-proline metabolism. Notably, spearman correlation analysis indicated that tryptophan, lysoPC (18:1/0:0), uric acid, and serotonin were strongly positively correlated with serum levels of both E 2 and PROG. Additionally, riboflavin, indoleacetic acid, and indole-3-propionic acid were positively correlated with E 2 levels. Our findings suggest that DHZCP may exert therapeutic effects primarily through the modulation of tryptophan and riboflavin metabolism, providing a solid foundation for its clinical application.
研究领域:
药理学
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妇产科学
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代谢组学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 5
·e70055
·
IF 1.7
Nan Guo,Sheng Hu,Yahui Zhang,Wen Zhang,Dejun Li,Yue Tang,Zijian Tai,Xin Guo,Bing Leng
Tigecycline has been widely used for treating infections caused by multidrug resistant bacteria, but the dosage and intrapulmonary distribution were still controversial. In this study, a UPLC–MS/MS method was established and fully validated to quantify tigecycline in human plasma and BALF. A simple and rapid protein precipitation was used to extract the analytes from plasma and BALF samples. Then, tigecycline and IS were separated on a SHIMADZU AQ-C18 column and detected using electrospray ionization positive ion mode using the transitions of m / z 586.3 → 513.2 m / z for TGC and 458.0 → 441.0 m / z for minocycline (IS). The linearity of the calibration was in the range of 20–2000 ng/mL in plasma and BALF. The validated method was successfully applied to investigate pharmacokinetic characteristics of tigecycline in critically ill patients. The results suggested that after intravenous administration of 100-mg q12h tigecycline, the AUC 0–12 was 3663.02 ± 2075.84 ng × h/mL and C ss,av was 305.25 ± 172.99 ng/mL; the average plasma concentration/ELF concentration ratio was 3.66. Significant individual differences and highly variable pharmacokinetic properties were observed, indicating that adjustment of dosing regimens according to therapeutic drug monitoring is effective and efficient to guarantee the drug efficacy and safety especially for critically ill patients.
研究领域:
临床医学
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药理学
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 5
·e70066
·
IF 1.7
Jiemei Liang,Hua Zhu,Qiyuan Yang,Zhouwei Li,Xiang Meng,Lanlan Fan,Li Li
Taxillus chinensis (DC) Danser ( T. chinensis ) is broadly used in traditional Chinese medicine. Although pharmacological research shows that the ethyl acetate extract of T. chinensis (JEA) has beneficial effects in treating hyperuricemic nephropathy (HN), the active components and potential mechanisms for these effects remain unclear. This study aims to predict the effective components and mechanism of JEA for HN. Firstly, we adopted UHPLC-Q-Exactive HFXMS technology to analyze the chemical profile of JEA and the absorbed prototype ingredients in rat plasma. In addition, network pharmacology methods were utilized by us to elaborate on the active compounds, signaling pathways, and potential mechanisms of JEA in treating HN. Finally, a UPLC method was established to screen potential chemicals that can effectively inhibit the activity of xanthine oxidase (XOD). A total of 92 components were systematically characterized in JEA. Of those, 46 compounds were identified in the plasma of rats administered with JEA extract. Through network pharmacology, 10 potential active components, 10 crucial target genes, and 20 pathways were predicted to be involved in the JEA-mediated treatment of HN. The molecular docking results indicated that oxyresveratrol, isorhammeiol, and robinetwere exhibited strong binding affinities for GAPDH, PPARG, and ALB. The analysis of the XOD inhibition experiment suggested that dihydromyricetin and oxyresveratrol exhibited potent inhibitory effects on XOD, with IC 50 values of 0.48 and 0.68 mg·mL −1 . This study preliminarily identified the potential effective components of JEA and revealed its underlying molecular mechanisms of action in preventing HN, which will improve our further studies on JEA to treat HN.
研究领域:
中药学
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药理学
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代谢组学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2024
·
IF 1.8
Ping Huang,Ting Xiang,Qiong Wang,Lintao Han,Sili Zheng,Dongning Zhang,Fang Huang,Bailu Duan,Jingjing Li,Huamao Li,Tao Huang
Xixin–Ganjiang herb pair (XGHP) is a classic combination for warming the lungs to dissolve phlegm and is often used to treat a variety of chronic lung diseases; it can treat the syndrome of cold phlegm obstruction of lungs. First, ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) was used to examine the composition of XGHP, and network pharmacology was used to predict its potential core targets and signaling pathways in the current study. Second, a rat model of chronic obstructive pulmonary disease (COPD) was established for assessing the anti-COPD activity of XGHP, and metabolomics was used to explore the biomarkers and metabolic pathways. Finally, the sample was validated using molecular docking and Western blotting. The integration of metabolomics and network pharmacology results identified 11 targets, 3 biomarkers, 3 pathways, and 2 metabolic pathways. Western blotting showed that XGHP effectively regulated the expression of core proteins via multiple signaling pathways (downregulation of toll-like receptor 4 [ TLR4 ] and upregulation of serine/threonine-protein kinase 1 [ p-AKT1 ] and nitric oxide synthase 3 [ NOS3 ]). Molecular docking results showed that the 10 potentially active components of XGHP have good affinity with tumor necrosis factor-alpha ( TNF-α ), interleukin-6 ( IL-6 ), matrix metalloproteinase 9 ( MMP-9 ), TLR4 , p-AKT1 , and NOS3 . Our findings suggest that XGHP may regulate glucolipid metabolism, improve energy supply, and inhibit inflammatory responses ( TNF-α , IL-6 , and MMP-9 ) via the PI3K-Akt signaling pathway and HIF-1 signaling pathway in the management of COPD.
研究领域:
药理学
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代谢组学
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网络药理学
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慢性阻塞性肺疾病
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中药学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 10
·e70136
·
IF 1.7
Yiyao Zhang,Guangyun Zhang,Fen Yang,Zhikang Zou
Hemoglobin A 1c (HbA 1c ) plays a role in the diagnosis and assessment of glycemic control in patients with diabetes. However, few studies have focused on the preparation methods and analytical performance evaluation of different formulations of mobile-phase buffers for HbA 1c assays. In this study, mobile-phase buffers of new formulations were prepared for the measurement of HbA 1c . Following the Clinical and Laboratory Standards Institute (CLSI) guidelines, the analytical performance of newly developed mobile-phase buffers was evaluated. The CVs of the intra- and inter-assay precision were less than 0.94%, the RDs of accuracy were less than ± 3.00%, and the carryover was 0.00%. The measured HbA 1c values were linear from 4.50% to 16.80% (26.00–160.00 mmol/mol). A comparison of newly developed and commercial mobile-phase buffers revealed that the Pearson regression equation was Y = 0.9862 x + 0.0888 ( R 2 = 0.9990), and the Bland–Altman mean difference between the two mobile-phase buffers was −0.02833% (95% CI: −0.1853% to 0.1278%). The chromatography column had a lifetime of over 7000 tests. The reference interval was 4.30%–6.30% (23.00–45.00 mmol/mol). Stability was acceptable within 24 months. The newly developed mobile-phase buffers demonstrated good analytical performance (i.e., precision, linearity, accuracy, carryover, reference interval, the number of chromatography column runs, and stability).
研究领域:
临床化学
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糖尿病诊断
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分析方法验证
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色谱分析
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2015
·Vol. 29
·期 12
·1834-1841
·
IF 1.723
Hua Fan,Chaozhan Wang,Yinmao Wei
Salbutamol (SAL) is the most widely used β 2 -agonist drug for asthma and chronic obstructive pulmonary patients, but it is also often abused as feed additive. In recent years, the abuse of SAL has led to a large number of food safety incidents. Therefore, the monitoring of SAL residues in animal products is very important. A highly selective boronate affinity magnetic adsorbent was synthesized and developed for detection of trace levels of SAL residues in pig tissue samples. The obtained Fe 3 O 4 @SiO 2 @FPBA(4-formylphenylboronic acid) magnetic adsorbent showed good adsorption ability to catechol and SAL, and then it was successfully applied as special magnetic solid-phase phase extraction adsorbent coupled with high-performance liquid chromatography (HPLC) for simultaneous isolation and determination of cis -diol compounds. The binding capacity of catechol and SAL reached 96 and 50 µmol/g, respectively. The method was successfully established for the detection of trace levels of SAL in pig tissue samples. The linear range extended from 0.32 to 800 µg/kg ( R 2 = 0.9994). The limit of detection of SAL was 0.19 µg/kg. The recoveries were satisfactory (89.5–108.0%) at three spiked levels with RSD between 2.1 and 11.3%. These results indicated that the method has potential for enrichment and detection of trace levels of SAL residual in animal food products. Copyright © 2015 John Wiley & Sons, Ltd.
研究领域:
分析化学
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食品安全
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药物检测
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2024
·
IF 1.8
Yonglin Ma,Yue Zhang,Yu Zhao,Jiwen Wang,Qianqian Hu,Lianlin Yang,Shuzhen Chen,Yong Diao,Hongliang Ma
In this study, an online antioxidant assay based on HPLC-ABTS was mainly developed for screening the antioxidants of flavonoids from Astragali Radix (AR), and comparing the antioxidant capacity between traditional decoction pieces (TDP) of AR and cell wall-broken decoction pieces (CDP) of AR. The experimental results showed that the overall antioxidant capacity of CDP of AR was about twice as much as that of TDP of AR, which was specifically expressed as the antioxidant capacity of the screened antioxidants extracted from CDP was equivalent to 1.9–5.1 times that of those extracted from TDP, and three antioxidants were successfully screened, which were calycosin-7-O-β-D-glucoside, calycosin, and formononetin. The method established in this study is characterized by high efficiency and accuracy, which can simultaneously accomplish the screening of antioxidant components and the comparison of antioxidant capacity between samples, and provides a new method for the quality evaluation of AR from the perspective of antioxidant activity.
研究领域:
中药学
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分析化学
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2024
·Vol. 38
·期 7
·e5887
·
IF 1.8
Shuai-nan Zhang,Qi Liu,Xu-zhao Li
Omics, bioinformatics, molecular docking, and experimental validation were used to elucidate the hepatoprotective effects, mechanisms, and active compounds of Shandougen (SDG) based on the biolabel-led research pattern. Integrated omics were used to explore the biolabels of SDG intervention in liver tissue. Subsequently, bioinformatics and molecular docking were applied to topologically analyze its therapeutic effects, mechanisms, and active compounds based on biolabels. Finally, an animal model was used to verify the biolabel analysis results. Omics, bioinformatics, and molecular docking revealed that SDG may exert therapeutic effects on liver diseases in the multicompound and multitarget synergistic modes, especially liver cirrhosis. In the validation experiment, SDG and its active compounds (betulinic acid and gallic acid) significantly improved the liver histopathological damage in the CCl 4 -induced liver cirrhosis model. Meanwhile, they also produced significant inhibitory effects on the focal adhesion pathway (integrin alpha-1, myosin regulatory light chain 2, laminin subunit gamma-1, etc.) and alleviated the associated pathological processes: focal adhesion (focal adhesion kinase 1)–extracellular matrix (collagen alpha-1(IV) chain, collagen alpha-1(VI) chain, and collagen alpha-2(VI) chain) dysfunction, carcinogenesis (alpha-fetoprotein, NH 3 , and acetylcholinesterase), inflammation (tumor necrosis factor alpha, interleukin-1 [IL-1], IL-6, and IL-10), and oxidative stress (reactive oxygen species, malonaldehyde, and superoxide dismutase). This study provides new evidence and insights for the hepatoprotective effects, mechanisms, and active compounds of SDG.
研究领域:
中药学
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生物信息学
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肝脏病学
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2024
·Vol. 38
·期 6
·e5861
·
IF 1.8
Jianjin Guo,Shaojing Liu,Yan Guo,Lu Bai,Chi-Tang Ho,Naisheng Bai
Fraxinus mandshurica (Oleaceae) is used as a traditional medicinal plant for the treatment of red eyes, menstrual disorders, excessive leucorrhea, chronic bronchitis and psoriasis. To perform chemical characterization of the secondary metabolites of F. mandshurica roots, bark, stems and leaves, 32 samples were collected from eight provinces in this study. A total of 64 chemical components were detected from four different parts of F. mandshurica by ultra-performance liquid chromatography–quadrupole time-of-flight mass spectrometry. Meanwhile, a total of nine secoiridoids were obtained by natural product chemical extraction, isolation and identification methods. Quantitative analysis by high-performance liquid chromatography–diode array detection–mass spectrometry showed the highest total content of secoiridoids in the bark, which is also consistent with the traditional medicinal parts. The results of methodological validation showed that the correlation coefficient ( R 2 ) values were all >0.9993, indicating a good linear range of the standard curve, while the relative standard deviations of precision, reproducibility and stability were <3%, and the spiked recoveries ranged from 98.22 to 102.27%, indicating that the experimental method was reliable and stable. In addition, fingerprinting and a heatmap were established to demonstrate the content trends of F. mandshurica more visually from different origins. Multivariate analysis, including principal component analysis and partial least squares discriminant analysis, was performed to determine the chemical characteristics of different parts of F. mandshurica , and six characteristic secoiridoids that could be used to distinguish different origins were screened. Finally, the inhibition of tyrosinase, α -glucosidase, acetylcholinesterase and pancreatic lipase activities by the nine characteristic compounds and extracts from different parts were investigated, and the results showed that they all exhibited different degrees of enzyme activity inhibition and thus have potential applications in whitening and blemish removal, hypoglycemia, anti-Alzheimer's disease and anti-obesity as a new source of natural enzyme activity inhibitors. This study establishes an identification and evaluation method applicable to phytochemistry of different origins, which is a guideline for quality control, origin evaluation and clinical application of traditional medicinal plants. This is also an unprecedented study on the identification of the chemical composition of different parts of F. mandshurica , characteristic compounds and the inhibition of enzyme activity of extracts from different parts.
研究领域:
药用植物学
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分析化学
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生物化学
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2024
·Vol. 39
·期 1
·e6055
·
IF 1.8
Jianhui Luo,Songshen Chen,WenYang Song,Yongtong Huang,Song Gao,Jiu Wang
Ethoxysanguinarine (ETSG), a benzophenanthridine alkaloid, exhibits diverse biological activities, including antibacterial, antifungal, anti-inflammatory, antioxidant, and anti-tumor effects. Despite these properties, limited research exists on ETSG in vivo pharmacokinetics due to its poor solubility and low bioavailability. In this study, we developed a rapid and specific UPLC-MS/MS method for ETSG bioanalysis. Sample preparation involved one-step protein precipitation using methanol and phellodendrine as an internal standard (IS). The Waters HSS T3 column (2.1 * 50 mm, 1.8 μM) employed a gradient elution with mobile phases A (2 mmol/L ammonium formate aqueous solution-formic acid [99.8:0.2, v/v]) and B (methanol-formic acid [99.8:0.2, v/v]). Mass analysis via Waters Q-mass spectrometer utilized positive scan mode and multiple reaction monitoring. ETSG and IS were detected at m/z 332.0 → 274.0 and 342.0 → 177.0, respectively, within 7.0 min. The method demonstrated excellent precision, accuracy, recovery, and stability, with a linear calibration curve (1.1–560 ng/mL) and strong correlation coefficient (0.9984). Successful pharmacokinetic evaluation in Sprague–Dawley rats included intravenous ETSG administration and intragastric ETSG nanoemulsion/suspension. This method enables steroidal saponin analysis from ETSG in biological samples.
研究领域:
药物分析
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生物化学
·
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）