BIOMEDICAL CHROMATOGRAPHY
·
2023
·Vol. 37
·期 8
·e5656
·
IF 1.8
Minmin Shen,Haiying Gu,Kai Deng,Zhongpeng Li,Yumei Yuan,Yangjin He,Yin Jin,Nengming Lin
Vancomycin (VAN) has a narrow therapeutic window and variable pharmacokinetic properties, which require timely monitoring of plasma concentration to adjust the dosage for better effectiveness. A sensitive and quantitative immunochromatographic method was developed to detect VAN in plasma. The linear response range of the method to detect plasma VAN was 1.25–50 μg/mL. The intra- and inter-assay coefficients were 4.68% and 8.81%, respectively, while the recovery was 89.10%–98.32%. The clinical comparative experiment results demonstrated a good correlation (r > 0.90) between the fluorescent immunochromatographic strip test and the mass spectrum. In this study, a simple, rapid, and high-sensitivity immunochromatographic method was established for detecting VAN, which helped establish the basis for further application of monitoring plasma concentration.
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BIOMEDICAL CHROMATOGRAPHY
·
2023
·Vol. 37
·期 5
·e5611
·
IF 1.8
Zhiyu Fan,Gangqiang Yang,Xinjie Wu,Yanan Yang,Jinfang Xu
Biflavonoids are naturally occurring compounds consisting of two flavonoid moieties that have received substantial attention from researchers. Although many kinds of biflavonoids are typically distributed in Selaginella uncinata with hypoglycemic effect, their anti- α -glucosidase activities are not yet clear. In this study, a ligand fishing strategy for fast screening of α -glucosidase inhibitors from S. uncinata was proposed. α -Glucosidase was first immobilized on Fe 3 O 4 magnetic nanoparticles (MNPs) and then the α -glucosidase–functionalized MNPs were incubated with crude extracts of S. uncinata to fish out the ligands. Furthermore, considering the similarity and easy confusion of the structures of biflavonoids, the fragmentation patterns of different types of biflavonoids were studied. Based on this, 11 biflavonoids ligands with α -glucosidase inhibitory activities were accurately and quickly identified from S. uncinata with ultra-high-performance liquid chromatography–quadrupole time-of-flight–tandem mass spectrometry. Furthermore, these ligands were confirmed to be potential inhibitors through the in vitro inhibitory assay and molecular docking.
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BIOMEDICAL CHROMATOGRAPHY
·
2023
·Vol. 37
·期 4
·e5578
·
IF 1.8
Pan Lv,Fei Zhu,Meiyan Lv,Jiaqi Bao,Linying Lv,Xiangwei Xu,Yi Tao
In this study, we used a serum metabolomics methodology based on GC coupled with MS (GC–MS) to investigate the liver-protective effects of raw and stir-fried semen of Hovenia dulcis in rats models of carbon tetrachloride–induced liver injury. Multivariate statistical analysis, such as principal component analysis and orthogonal partial least squares discriminant analysis, were performed to examine changes in the metabolic state of rats with carbon tetrachloride–induced liver injury, as well as the recovery pattern of rats pretreated with the raw and stir-fried semen of H. dulcis . Liver tissues were subjected to histopathological examination. A total of 47 biomarkers were predicted to contribute to the dynamic pathological processes in the liver injury, such as phenylalanine, glutamic acid, glycine, arachidonic acid and linoleic acid. Further analysis revealed that pathways associated with phenylalanine, tyrosine and tryptophan biosynthesis, and linoleic acid metabolism were altered in the injured liver, and that pretreatment with raw and stir-fried semen of H. dulcis abolished the changes in the aforementioned metabolic pathways.
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BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 33
·期 12
·e4688
·
IF 1.748
MingNa Sun,Lu Yu,Zhou Tong,Xu Dong,Yue Chu,Mei Wang,TongChun Gao,JinSheng Duan
Phenamacril is a new broad-spectrum fungicide that is commonly used for the control of fungal diseases in wheat and rice. In this study, ultra-high-performance liquid chromatography–tandem mass spectrometry was used to establish a method for analyzing the residual phenamacril in flour and rice based on the improved QuEChERS ( qu ick, e asy, ch eap, e ffective, r ugged and s afe) method using Z-Sep+ as the adsorbent in the pre-treatment process. The average recovery of phenamacril in flour and rice was 82.2–96.0%, the relative standard deviation was 2.1–5.6% and the limit of quantification was 0.5 μg/kg. The accuracy and sensitivity of this method meet the requirements for residue analysis. The method was applied to commercially available flour and rice samples, and the detected concentrations of phenamacril were 0.005–0.033 mg/kg. This method provides technical support for the safety evaluation of phenamacril.
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BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 33
·期 9
·e4555
·
IF 1.748
Ke-ke Cui,Yue-ting Cao,Jia-feng Shao,Zheng-yu Lu,Long-hu Wang
Bufadienolides are the main bioactive components of Venenum Bufonis (VB) and have been widely used to treat different types of human cancers for decades. The bufadienolide content in VB varies significantly in materials from different geographical origins. In this work, a new strategy for the quality assessment of VB was developed through quantitative analysis of multi-components by single marker (QAMS). Cinobufagin was selected as the internal reference substance; seven bufadienolides were separated and simultaneously determined based on relative correction factors. The correlation coefficient value ( r ≥ 0.9936) between QAMS and the normal external standard method proved the consistency of the two methods. According to the outcomes of 30 batches of VB samples, the contents of the seven bufadienolides were used for further chemometric analysis. All of the samples of VB from various geographical origins were divided into three categories based on hierarchical cluster analysis and radar plot, which indicated the crucial influence of geographical origins on VB. This study showed that QAMS combined with chemometristry could be used to comprehensively evaluate and effectively control the quality of VB from different geographical origins.
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BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 33
·期 4
·e4454
·
IF 1.688
Jing-Xian Zhang,Mei-Juan Qi,Mei-Zhi Shi,Jun-Jun Chen,Xiang-Qi Zhang,Jiao Yang,Ke-Zhi Zhang,Yong-Long Han,Cheng Guo
Danhong injection (DHI) is made from Salvia miltiorrhiza Bunge. and Carthamus tinctorius L. extract and is widely used in the clinical treatment of cardiovascular and cerebrovascular diseases. This study aimed to evaluate the effect of DHI on cytochrome P450 (CYP450) enzymes in vitro to predict drug–drug interactions based on CYP450 as combination therapy. To assess the inhibitory effect of DHI on CYP450, we detected the IC 50 value of DHI on CYP450 in vitro by liquid chromatography/tandem mass spectrometry (LC–MS/MS). Simultaneously, the induction effect of DHI on CYP450s was also evaluated. The relative induction ratios of DHI on CYP1A2, CYP2B6 and CYP3A4 activity were calculated by LC–MS/MS. The expression level of CYP3A4 mRNA was determined by reverse transcription PCR (RT-PCR). The LC–MS/MS data showed DHI intensively inhibit CYP2A6 activity and the intensity of inhibition was followed by CYP2C8, CYP3A4, CYP2C19, CYP2B6, CYP2D6, CYP1A2, CYP2E1 and CYP2C9 in vitro . The results of RT-PCR showed that there is a certain induction of DHI on CYP3A4 mRNA in human primary hepatocytes in vitro . The study suggested that drug–drug interactions might occur in clinical co-administration of drugs owing to the CYP2A6 inhibition and CYP3A4 induction.
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BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 33
·期 9
·e4568
·
IF 1.748
Liping Zhou,Hexiang Liu,Zhongyong Xu,Su Guan,Lei Zhang
Febuxostat is a novel nonpurine type of highly selective xanthine oxidoreductase inhibitor. A rapid and sensitive ultra-high-performance liquid chromatography–quadrupole time-of-flight mass spectrometry method for simultaneous separation and determination of febuxostat and its metabolites in rat serum and urine was developed at various time points after oral administration to the rats. The febuxostat metabolites were predicted by biotransformation software and transformed to a personal compound database to quickly determine the possible metabolites from the MS1 data. The possibility of the MS/MS fragmentation was calculated by the Molecular Structure Correlator software. As a result, five phase I and two phase II metabolites in rat serum, and seven phase I and three phase II metabolites in rat urine were identified, of which four metabolites (M2, M5, M6, M7) have not been reported before. The metabolite toxicities are predicted, and the results are helpful for the design of new xanthine oxidoreductase inhibitors.
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BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 6
·e4210
·
IF 1.688
Weiguo Liao,Xiaojie Huang,Yongxin Yin,Bin Liu,Runzhi Zhu
Tetramethylpyrazine (TMP) has been widely used in the treatment of ischemic cerebrovascular disease. However, the mechanism of TMP and how to increase its bioavailability need to be further explored. In our study, an in vivo microdialysis sampling technique coupled with ultra-performance liquid chromatography–mass spectrometry method was developed to investigate the pharmacokinetic properties of TMP and its interaction with different doses of borneol (BO) in rats. Linearity of TMP in brain and blood dialysates exhibited good linear relationships over the concentration range of 0.991–555.14 ng/mL. The specificity, linearity, accuracy, precision, matrix effect and stability were within acceptable ranges. The results demonstrated that BO had a marked impact on the pharmacokinetic properties of TMP. After co-administration, the areas under the concentration–time curve (AUC) of TMP in brain and blood were significantly increased. Meanwhile, the peak concentration of TMP in brain was also enhanced. The AUC Brain /AUC Blood of TMP, increased from 44% to 56 and 60.8% after co-administration with BO (15 and 30 mg/kg). The pharmacodynamic results showed that TMP co-administration with BO enhanced the cerebral blood flow during the period of ischemia and reduced the infarct volume. Overall, it might be an effective way to treat stroke to use TMP co-administered with BO.
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BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 6
·e4192
·
IF 1.688
Dan Li,Gang Zhao,Weipeng Ai,Gao Li,Luqin Si,Jiangeng Huang,Yunzhou Chen,Sanlan Wu
In this study, a liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed and validated to simultaneously determine the anticancer drugs etoposide and paclitaxel in mouse plasma and tissues including liver, kidney, lung, heart, spleen and brain. The analytes were extracted from the matrices of interest by liquid–liquid extraction using methyl tert -butyl ether–dichloromethane (1:1, v/v). Chromatographic separation was achieved on an Ultimate XB-C 18 column (100 × 2.1 mm, 3 μm) at 40°C and the total run time was 4 min under a gradient elution. Ionization was conducted using electrospray ionization in the positive mode. Stable isotope etoposide-d3 and docetaxel were used as the internal standards. The lower limit of quantitation (LLOQ) of etoposide was 1 ng/g tissue for all tissues and 0.5 ng/mL for plasma. The LLOQ of paclitaxel was 0.4 ng/g tissue and 0.2 ng/mL for all tissues and plasma, respectively. The coefficients of correlation for all of the analytes in the tissues and plasma were >0.99. Both intra- and inter-day accuracy and precision were satisfactory. This method was successfully applied to measure plasma and tissue drug concentrations in mice treated with etoposide and paclitaxel-loaded self-microemulsifying drug-delivery systems.
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BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 6
·e4193
·
IF 1.688
Ping Guo,Jingjing Zhang,Xiaohui Chen,Longshan Zhao
A molecularly imprinted polymer was synthesized and applied as a sorbent in the solid-phase extraction device. The imprinted polymer was characterized by fourier-transform infrared spectroscopy and scanning electron microscope. The results revealed that imprinted polymer possess sensitive selectivity and reliable adsorption properties for five NSAIDs. The imprinted polymer was successfully applied to the pre-concentration for five NSAIDs in different water samples prior to UPLC-MS/MS. In the early studies, several factors were investigated, including pH adjustment, the kind of elution solvent and the volume of elution solvent. Finally, we found that the pH 5 and an aliquot of 2 mL methanol were suitable for the water samples. The limits of detection and limits of quantitation of five nonsteroidal anti-inflammatory drugs varied from 0.007 to 0.480 μg L −1 and 0.03 to 1.58 μg L −1 , respectively. The spiking recoveries of the target analytes were 50.33-127.64% at the levels of 0.2 μg L −1 , 2 μg L −1 and 5 μg L −1 . The precision and accuracy of this method showed a great increase compared with traditional solid-phase extraction. The developed method was successfully applied to extraction and analysis of NSAIDs in different water samples with satisfactory results which could help us better understand their environmental fate and risk to ecological health.
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BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 11
·e4338
·
IF 1.688
Dan Huang,Qing-Song Jiang,Jun-Qing Yang,Ting Cui,Nian-Ru Wang,Ting-Ting Du,Xin-Hui Jiang
The determination of amino acids and monoamine with actions like neurotransmitters or modulators has become increasingly important for studying the relationship between the dysfunction of neurotransmitters and the pathogenesis of diabetic encephalopathy. Here, a high-performance liquid chromatography with fluorescence detection method was developed to simultaneously determine nine monoamines and amino acids including three excitatory neurotransmitters (aspartate, glutamate, and serotonin), four inhibitory neurotransmitters (glycine, γ -aminobutyric acid, taurine, dopamine), a precursor of 5-HT (tryptophan) and methionine using homoserine as the internal standard. The separation was performed on a BDS column with methanol-buffer solution of 35 mmol/L sodium acetate and 5 mmol/L citric acid (pH 6.0) using a simple gradient elution. Several parameters including specificity, precision, and recovery were validated after optimization of the analytical conditions. The developed method was successfully applied to determine the cortex and the hippocampus samples from Sprague–Dawley rats. Our results showed that various neurotransmitters involved in diabetes mellitus may tend to be differentially modulated and present a different alteration tendency at different time course, which might be associated with the duration of diabetes mellitus.
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BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 10
·e4306
·
IF 1.688
Jie Yang,Zhi Sun,Duolu Li,Fei Duan,Zhuolun Li,Jingli Lu,Yingying Shi,Tanye Xu,Xiaojian Zhang
Shenkang injection is a traditional Chinese formula with good curative effect on chronic renal failure. In this paper, a novel, rapid and sensitive ultra-high-performance liquid chromatography coupled with Q Exactive hybrid quadrupole Orbitrap high-resolution accurate mass spectrometry was developed and validated for simultaneous determination of seven bioactive constituents of Shenkang injection in rat plasma and tissues after intravenous administration. Acetonitrile was used as a protein precipitation agent in biological samples disposal with carbamazepine as internal standard. The chromatographic separation was carried out on a C 18 column with a gradient mobile phase consisting of acetonitrile and water (containing 0.1% formic acid). The MS analysis was performed in the full-scan positive and negative ion mode. The lower limits of quantification for the seven analytes in rat plasma and tissues were 0.1–10 ng/mL. The validated method was successfully applied to tissue distribution and pharmacokinetic studies of Shenkang injection after intravenous administration. The results of the tissue distribution study showed that the high concentrations of seven constituents were primarily in the kidney tract. This is the first report of the application of Q-Orbitrap with full-scan mass spectrometry in tissue distribution and pharmacokinetic studies of Shenkang injection.
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