BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 34
·期 3
·e4748
·
IF 1.748
Chu Liu,Xiangyong Yu,Zhaorui Meng,Ning Zhao,Fujuan Bai,Longshan Zhao
A simple and efficient method involving microwave-assisted extraction (MAE) combined with GC–MS was established to determine 1,3-di- tert -butylbenzene (DBB), 2,4-di- tert -butylphenol (DBP), 3,5-di- tert -butyl-4-hydroxybenzaldehyde (DBHBA) for evaluating the compatibility of antimicrobial peptide PL-5 spray with drug-packaging materials. In this study, the antimicrobial peptide PL-5 spray was purified using a Welchrom C18 column, and the high-density polyethylene spray bottle with liquid collection tube was first mixed with absolute ethanol, which would be subjected to MAE for further measurement by GC–MS. Various experimental parameters were systematically optimized, and good linearities were obtained within the range of 0.05–1.00 μg/mL for DBB and DBHBA and 0.50–10.00 μg/mL for DBP, with limits of detection (LODs) of 0.99 ng/mL (DBB), 16.34 ng/mL (DBP), and 1.64 ng/mL (DBHBA). Satisfactory recoveries that ranged from 96.0% to 107.2% were acquired, and the relative standard deviation was ≤ 4.7%. The results showed that the maximum daily usage of DBB, DBP, and DBHBA was 9.859, 163.445, and 16.399 ng, respectively, which was far below the corresponding permitted daily exposure values according to the safety assessment, indicating that the migration of analytes did not bring any potential safety risk. The compatibility between the drug and the packaging materials was favorable.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 34
·期 3
·e4773
·
IF 1.748
Lili Li,Shuangshuang Ma,Daijie Wang,Long Chen,Xiao Wang
Lonicerae Japonicae Flos (LJF) is a typical herbal medicine and is used as a functional food. LJF, which has complex chemical compounds, has various biological effects. The global metabolomics, focusing on both the endogenous and exogenous metabolites, have not yet been investigated for LJF in normal healthy rats using LC–MS. In this study, plasma metabolomics was analyzed after the administration of LJF at different time intervals, and the exogenous metabolites were identified. Partial least squares discriminant analysis showed significant differences in chemical content in the dosed rats. Cholic acid, indoleacrylic acid, indolelactic acid, hippuric acid, N -acetyl-phenylalanine, and N -acetyl-serotonin significantly accumulated in the dosed rats. Lysophosphatidylethanolamine and lysophosphatidylcholine content, including plasmalogen, increased. There were 25 components of LJF, including 15 prototypes and 10 metabolites, that were identified. The 15 prototypes included phenolic acids, flavonoids, and iridoids, and their contents decreased with an increase in the administration time. Glucuronidation and sulfation of polyphenols were found for LJF. The exogenous glucuronide and sulfate metabolites—including dihydrocoumaric acid-sulfate, dihydrocaffeic acid-sulfate, dihydroferulic acid-sulfate, apigenin-glucuronide, apigenin-glucuronide-sulfate, isorhamnetin-glucuronide-sulfate, and others—were identified with a neutral loss of 176 and 80, respectively. The metabolic differences found in the study may serve as biomarkers of LJF consumption and promote the understanding of the mechanism of action of LJF.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 34
·期 3
·e4767
·
IF 1.748
Yong-hong Liu,Ting-ting Du,Jing-yuan Wan,Hua Zhao,Dan Huang,Jian-sha Li,Xin-hui Jiang
Disorders of certain branched-chain amino acids may be associated with the occurrence and development of non-alcoholic fatty liver disease. Measurement of related branched-chain amino acid levels could provide a reference for the clinical and scientific research of the non-alcoholic fatty liver disease. An established HPLC–FLD method was used to quantify aspartic acid, glutamate, glutamine, glycine, taurine, tyrosine, 4-amino butanoic acid, tryptophan, methionine, valine, phenylalanine, isoleucine and leucine in mouse brain tissue. Brain tissue samples mixed with internal standard (3-aminobutyric acid) were processed, then derivatized with 2- O -phthaldialdehyde, and finally separated on an ODS2 column through gradient elution at a flow rate of 1.0 ml·min −1 . The excitation and emission wavelengths were set at 340 and 455 nm, respectively. The mobile phase A was 100% methanol and the mobile phase B consisted of 30 mmol·L −1 sodium acetate (pH 6.8). The injection volume was 20 μl and the single run time was 45 min. Several parameters, accuracy, precision, and stability, were verified and the results showed the established method had good sensitivity and resolution for all of the 13 compounds and internal standard in mouse brain.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2019
·Vol. 34
·期 2
·e4763
·
IF 1.748
Qing-ling Qi,Ya-Ming Yu,Cheng Tang
Target biomolecule-immobilized magnetic beads could be used as a powerful tool for screening active compounds present in natural products. Low damage rates of the target proteins, associated with the availability of diverse automated online approaches for analysis, make it a valuable tool for affinity studies. RAW264.7 cells (a kind of murine macrophage cell line) were used in this study. These cellular membranes were immobilized onto the surface of MBs and were used for screening the active compounds of Polygonatum sibiricum. Combining this technique with HPLC led to the identification of an active compound and its biological activity was confirmed. This is the first report establishing the use of RAW264.7 cellular membrane-coated magnetic bead fishing followed by HPLC analysis for screening active compounds from natural products.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2024
·Vol. 39
·期 1
·e6050
·
IF 1.8
Tiantian Xie,Yanling Hao,Yanzheng Xie
Methylophiopogonanone A (MOA) is one of the homoisoflavonoids isolated from Ophiopogon japonicus , which has been demonstrated to have extensive pharmacological activities. The aim of this study was to develop and validate a liquid chromatography–tandem mass spectrometry method for the measurement of MOA in rat plasma. Methylophiopogonanone B (MOB) was used as internal standard. After precipitation with acetonitrile, the samples were separated using a Waters ACQUITY HSS T 3 column with 0.1% formic acid solution and acetonitrile as mobile phase. Mass detection was monitored using multiple reactions monitoring mode with precursor-to-product ion transition of m/z 343.2 > 135.1 for MOA and m/z 329.2 > 121.1 for internal standard. The assay showed good linearity over the concentration range of 1–1000 ng/mL, with correlation coefficient > 0.997. The lower limit of quantification (LLOQ) was 1 ng/mL. Acetonitrile-mediated precipitation showed high extraction efficiency (> 80%). The accuracy and precision were within the acceptable limits. MOA was demonstrated to be stable in rat plasma under the tested storage conditions. After validation, the proposed method was applied to the pharmacokinetic study of MOA in rat plasma, and the data revealed that MOA showed rapid absorption and elimination from rat plasma. The oral bioavailability of MOA in rat was 24.5%.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 3
·e6090
·
IF 1.7
Fang Wang,Wenfei Sun,Zheheng Ma,Furui Chu
Proteolysis targeting chimera (PROTAC) has been developed and currently enjoys widespread interest among the field of pharmaceutical manufacturing in recent decades. NX-5948 is an orally active PROTAC Bruton tyrosine kinase degrader, which shows anti-inflammatory and antitumor activities. In this study, a simple and fast bioanalytical method for the quantification of NX-5948 in beagle dog plasma was developed using liquid chromatography–tandem mass spectrometry (LC-MS/MS). A full method validation was performed according to regulatory guidelines. For the quantification, [M + H] + was formed using an electrospray ionization (ESI) source in the positive ion mode, and selective reaction monitoring (SRM) was employed using a triple quadrupole mass spectrometry. The monitored precursor-to-product transitions were m/z 807.5 > 790.5 for NX-5948 and m/z 812.4 > 452.1 for internal standard. A linear response was obtained at the concentration range of 0.5–200 ng/mL, with correlation coefficient > 0.99. The interday accuracy ranged from −9.03% to 5.99% (RSD < 7.84%), and the intraday accuracy from −5.15% to 8.56% (RSD < 6.90%). NX-5948 was demonstrated to be stable under the present storage conditions. After validation, the method was successfully applied for the quantification of NX-5948 in beagle dog plasma after oral and intravenous administration of the NX-5948.
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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.
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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.
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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.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2015
·Vol. 30
·期 1
·75-80
·
IF 1.723
Congcong Wen,Zhiyi Wang,Meiling Zhang,Shuanghu Wang,Peiwu Geng,Fa Sun,Mengchun Chen,Guanyang Lin,Lufeng Hu,Jianshe Ma,Xianqin Wang
Paraquat is quick-acting and non-selective, killing green plant tissue on contact; it is also toxic to human beings and animals. In this study, we developed a urine metabonomic method by gas chromatography–mass spectrometry to evaluate the effect of acute paraquat poisoning on rats. Pattern recognition analysis, including both partial least squares discriminate analysis and principal component analysis revealed that acute paraquat poisoning induced metabolic perturbations. Compared with the control group, the levels of benzeneacetic acid and hexadecanoic acid of the acute paraquat poisoning group (intragastric administration 36 mg/kg) increased, while the levels of butanedioic acid, pentanedioic acid, altronic acid decreased. Based on these urinary metabolomics data, support vector machine was applied to discriminate the metabolomic change of paraquat groups from the control group, which achieved 100% classification accuracy. In conclusion, metabonomic method combined with support vector machine can be used as a useful diagnostic tool in paraquat-poisoned rats. Copyright © 2015 John Wiley & Sons, Ltd.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2015
·Vol. 29
·期 9
·1406-1414
·
IF 1.723
Zheng Tang,Ran Yin,Kaishun Bi,Heyun Zhu,Fei Han,Kelin Chen,Fenrong Wang
Zhi-Zi-Da-Huang decoction (ZZDHD), a classical traditional Chinese medicine (TCM) prescription composed of four herbal medicines, has been widely used in treating various hepatobiliary disorders for a long time. The objective of this study was to develop a sensitive and efficient liquid chromatography coupled with mass spectrometry (LC-MS) method for quantitative determination of 20 active constituents, including three iridoid glycosides, 11 flavonoids, three anthraquinones and three tannins in ZZDHD. Separation was achieved on a phenomenex kinetex C 18 column (150 × 4.6 mm, 2.6 µm) using gradient elution with a mobile phase consisting of acetonitrile and 0.1% formic acid in water. Detection was performed with electrospray ionization source in the negative ionization and selected ion monitoring mode. The established method was validated by determining the linearity ( r 2 ≥ 0.9983), limit of quantification (0.16–300 ng/mL), precision (RSD ≤ 4.6%), average recovery (96.0–105.6%), repeatability (RSD ≤ 3.2%) and stability (RSD ≤ 4.5%). Then, the method was successfully applied to investigate the chemical composition variations owing to the interaction between the four component herbs of ZZDHD during the extraction process. It was found that different combinations of the herbs affect the extraction efficiency of chemical constituents in different ways. The validated LC-MS method provides a meaningful basis for quality control and further research on ZZDHD. Copyright © 2015 John Wiley & Sons, Ltd.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2016
·Vol. 30
·期 11
·1796-1806
·
IF 1.729
Junjun Ni,Li Xu,Wei Li,Lijun Wu
Easy-to-use early cancer detection methods based on metabolomics using serum samples have been developed recently. Among metabolites, amino acids and acylcarnitine are two of the most suitable candidates for diagnosing lung cancer. The purpose of the present study was to develop a novel, sensitive and specific liquid chromatography–tandem mass spectrometry (LC–MS/MS) method to simultaneously determine 13 amino acids and 8 acylcarnitines in lung cancer patients in serum. After derivatization, the 21 analytes were separated using a C 18 column with gradient elution program in 14 min, obtaining recovery within 90.4–113.8% and precision within 0.3–14.8%. The method was successfully applied in concentration determination of lung cancer patients and healthy controls. The results showed that the serum concentration of lung cancer patients were significant from those of healthy controls.
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