BIOMEDICAL CHROMATOGRAPHY
·
2023
·Vol. 37
·期 12
·e5743
·
IF 1.8
Wei-Han Yang,Jing-Wen Hao,Nai-Dong Chen,Jiao Li
The determination of monosaccharides is crucial for studying the structure of polysaccharides and the composition of free monosaccharides in living organisms. Based on previous derivatization gas chromatography–mass spectrometry (GC–MS) methods, we aimed to develop a novel analytical protocol for better quantifying monosaccharides. In this study, sugar alcohol acetylation, saccharonitrile acetylation, silylation and a combination of sugar alcohols acetylation and saccharonitrile acetylation were compared. The optimal method was verified with the monosaccharide determination of four polysaccharides and four free monosaccharides from Dendrobium . The results showed that the novel combined derivatization method was superior to the other three methods in terms of content analysis of monosaccharides. Furthermore, it possessed good linearity (all calibration curves showed relative coefficients ≥ 0.999), sensitivity, precision (relative standard deviation < 2%), and accuracy (recovery, 95.7–105%). Finally, the novel method established in this study was successfully employed in determining the monosaccharide composition of four polysaccharides and four free monosaccharide samples from Dendrobium .
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2021
·Vol. 35
·期 6
·e5084
·
IF 1.902
Jian-Sha Li,Hong-mei Qiu,Qing-song Jiang,Yong-hong Liu,Jing Zhang,Tao Gong,Xin-hui Jiang
Emerging evidence suggests that amino acid (AA) neurotransmitters play important roles in the pathophysiological processes of cerebral ischemia. In this work, an HPLC with fluorescence detection (HPLC-FLR) method was developed for the simultaneous determination of 18 AAs in the cortex and plasma after cerebral ischemia in mice. The ischemia model was prepared by bilateral common carotid artery occlusion, and then the cortex and plasma of the sham, ischemia, and naringenin groups were collected. Based on the protein precipitation method, a simple and effective sample preparation method was developed. The treated sample contained minimal proteins and lipids. The analysis of the sample was performed by the proposed HPLC-FLR method in combination with o -phthalaldehyde. The results showed a statistically significant increase in excitatory AAs (aspartic acid and glutamic acid), inhibitory AAs (glycine and 4-aminobutyric acid), phenylalanine, citrulline, isoleucine, and leucine levels, and a decrease of glutathione and phenylalanine levels when compared with the sham group in the cortex. Besides, the administration of naringenin had significant effects on excitatory AAs, inhibitory AA (glycine), glutamine, tyrosine, phenylalanine, and leucine levels when compared with the sham group in the cortex. These findings could be utilized in studying and clarifying the mechanisms of ischemia.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2021
·Vol. 35
·期 10
·e5172
·
IF 1.902
Cancan Duan,Weina Cheng,Qihong Chen,Xiaofei Li,Jianyong Zhang
A sensitive gas chromatography–mass spectroscopy method was established for the determination of cantharidin (CTD) in rat plasma and liver homogenates. During the experiment, rats were randomly divided into two groups (low, high) and were administered aqueous extract of Mylabris compound for 7 days. Then, plasma and tissue samples were taken at different time points to study the pharmacokinetics and tissue distribution of CTD in rats. The selected reaction monitoring transitions for CTD and clofibrate (internal standard) were m / z 128 → 85 and m / z 169 → 141, respectively. The calibration curve ranged from 10.26 to 3,078 ng/ml for plasma and from 10.26 to 246.24 ng/ml for liver homogenates. The lower limits of quantification were 10.26 ng/ml for both plasma and liver. The intra- and inter-day precision and accuracy were <20% for both plasma and liver homogenates. Extraction recovery ranged from 89.21 to 103.61% for CTD in rat plasma and liver and from 83.79 to 102.74% for IS in rat plasma and liver. Matrix effects ranged from 93.06 to 110.44% for CTD and from 91.65 to 110.80% for IS.
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BIOMEDICAL CHROMATOGRAPHY
·
2021
·Vol. 35
·期 7
·e5093
·
IF 1.902
Wei Wu,Rui Cheng,Zhenzhou Jiang,Luyong Zhang,Xin Huang
A rapid and specific UPLC–MS/MS method with a total run time of 3.5 min was developed for the determination of pravastatin, fexofenadine, rosuvastatin, and methotrexate in rat primary hepatocytes. After protein precipitation with 70% acetonitrile (containing 30% H 2 O), these four analytes were separated under gradient conditions with a mobile phase consisting of 0.03% acetic acid (v/v) and methanol at a flow rate of 0.50 mL/min. The linearity, recovery, matrix effect, accuracy, precision, and stability of the method were well validated. We evaluated drug–drug interactions based on these four compounds in freshly suspended hepatocytes. The hepatic uptake of pravastatin, fexofenadine, rosuvastatin, and methotrexate at 4°C was significantly lower than that at 37°C, and the hepatocytes were saturable with increased substrate concentration and culture time, suggesting that the rat primary hepatocyte model was successfully established. Triptolide showed a significant inhibitory effect on the hepatic uptake of these four compounds. In conclusion, this method was successfully employed for the quantification of pravastatin, fexofenadine, rosuvastatin, and methotrexate and was used to verify the rat primary hepatocyte model for Oatp1, Oatp2, Oatp4, and Oat2 transporter studies. Then, we applied this model to explore the effect of triptolide on these four transporters.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2021
·Vol. 35
·期 6
·e5076
·
IF 1.902
Kaiyang Wang,Lan Luo,Xiaoli Xu,Xingyu Chen,Qiong He,Zhongjie Zou,Shumei Wang,Shengwang Liang
Dyspepsia, one of the most prevalent diseases of the digestive tract that impacts the quality of patient life, is mainly caused by gastrointestinal motility disorder. Hawthorn is a commonly used traditional Chinese medicine for treating dyspepsia, and has been proven to improve gastrointestinal motility. Herein, a rat model of gastrointestinal motility disorder was established by subcutaneous injection with atropine. The modeled rats were treated with four polar parts (T1–4 in descending polarity, corresponding to water, n -butanol, ethyl acetate and petroleum ether extracts, respectively) of hawthorn. Through metabolomics analysis, a total of 20 significantly metabolites were identified with significant changes in their abundance levels and these metabolites were related to many metabolic pathways such as amino acid metabolism and primary bile acid biosynthesis. The results showed that T3 had the best therapeutic effect of promoting gastrointestinal motility. Other parts showed no obvious therapeutic effect, demonstrating that the effective components of hawthorn may be compounds of medium polarity. T3 might achieve good therapeutic effects owing to the gastrointestinal motility promotion activity, and by rectifying the disturbed metabolic pathways in the gastrointestinal motility disorder model.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2020
·Vol. 35
·期 3
·e4991
·
IF 1.728
Li-Juan Nie,Jun Liang,Feng Shan,Ya-Yun Xu,Chun-Yu Yan,Xuan Zhou,Zhuo-Yu Cheng,Qing-Rong Xia
A simple, rapid, and selective ultra-performance liquid chromatography–tandem mass spectrometry method for determination of l -carnitine (LC) and acetyl- l- carnitine (ALC) in human serum was developed. Acetyl- l- carnitine-d 3 (ALC-d 3 ) was selected as internal standard (IS). After protein precipitation with acetonitrile–water (1 mL, 2:1, v/v), the analytes and IS were separated on a 2.5-μm XSelect HSS T3 C 18 column by gradient elution with methanol–water (containing 0.01% ammonia water) as the mobile phase at a flow rate of 0.2 mL/min. Analytes were detected with multiple reaction monitoring using a positive scan mode with electrospray ionization. Good linearity ( R 2 > 0.999) was observed in the concentration range for LC and ALC. The inter- and intra-day values of relative error were −10.4% to 10.0% with CVs less than 9.84%. The average recoveries of the two analytes were 91.29%–98.23%. Blood samples containing LC and ALC were stable under various storage conditions. Normal, haemolytic, and hyperlipidaemic serum had no significant effect on the quantification of LC and ALC. This method was successfully applied to study the concentrations of endogenous LC and ALC in the serum of patients with first-episode depression.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2020
·Vol. 34
·期 10
·e4919
·
IF 1.728
Xinchi Feng,Kun Wang,Xintong Hu,Liwei Chai,Shijie Cao,Liqin Ding,Feng Qiu
Rhizoma coptidis has been used for a long time in China owing to its anti-bacterial, anti-diabetes, anti-hyperlipidemia and anti-obesity activities. However, the in vivo biotransformation of Rhizoma coptidis is still unclear to date. In this study, a three-step strategy using UPLC-Q-TOF/MS was applied to clarify the in vivo absorbed constituents and metabolites in rats after oral administration of Rhizoma coptidis. First, alkaloids in Rhizoma coptidis extract were identified. Second, six abundant alkaloids (berberine, palmatine, coptisine, epiberberine, jatrorrhizine, and columbamine) were selected as representative prototypes and the metabolic fates of them in rats were investigated to obtain a database of Rhizoma coptidis -derived metabolites. Finally, the metabolic profiles of Rhizoma coptidis were fully elucidated based on the above-mentioned results. In summary, 29 alkaloids were identified in Rhizoma coptidis , and a database of Rhizoma coptidis -derived metabolites was obtained with 144 characterized metabolites. A total of 89 xenobiotics including 12 absorbed constituents and 77 metabolites were identified in dosed rat biosamples. Major metabolic pathways of Rhizoma coptidis were hydroxylation, reduction, methylation, demethylation, demethylenation, desaturation, glucuronidation and sulfation. This is the first systematic study on the in vivo absorbed constituents and metabolic profiling of Rhizoma coptidis and will be beneficial for its further studies.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2020
·Vol. 34
·期 9
·e4870
·
IF 1.728
Jiping Yi,Bin Chen,Yongzheng Bao,Jingyu Wang
In this study, a simple and reliable LC–MS/MS method was first proposed for the simultaneous determination of TUG-891 and its metabolites TUG-891-alcohol, TUG-891-aldehyde, and TUG-891-acid in rat plasma. The analytes and fasiglifam (internal standard) were extracted from plasma samples with acetonitrile and separated using an Acquity BEH C 18 column (1.7 μm, 2.1 × 50 mm) with water containing 0.05% ammonium hydroxide and acetonitrile containing 0.05% ammonium hydroxide as the mobile phase. A Q-Exactive Orbitrap mass spectrometer in full-scan mode was used for mass detection, and the data analysis was obtained using a mass extraction window of 5 ppm. The calibration curves exhibited excellent linearity (correlation coefficient > 0.9981) in the concentration range of 0.5–1000 ng/mL. The lower limit of quantification was 0.5 ng/mL for all analytes. The intra- and inter-day precision was less than 11.31%, and the accuracy ranged from −11.50 to 9.50%. The extraction recovery of the analytes from rat plasma was greater than 82.31%, and no obvious matrix effect was found. The established method was further applied to the pharmacokinetic study of TUG-891, TUG-891-alcohol, TUG-891-aldehyde, and TUG-891-acid in rat after a single dose of 5-mg/kg treatment of TUG-891. The results demonstrated that TUG-891 was rapidly metabolized into its metabolites and the systemic exposures of the metabolites were much higher than those of TUG-891.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2020
·Vol. 34
·期 8
·e4852
·
IF 1.728
Jing Wang,Yong Zhang,Meiqi Zhou,Meizhu Zheng,Jing Cui,Zhiqiang Liu,Chunming Liu,Shu Liu
Superoxide anion radical scavenger and xanthine oxidase inhibitor play an important role in the treatment of several relevant human diseases. In the present study, ultrafiltration liquid chromatography–mass spectrometry coupled to microplate reader was applied to screen and identify superoxide anion radical scavengers and xanthine oxidase inhibitors from total flavonoids of Ginkgo biloba leaves. As a result, four compounds (quercetin, apigenin, kaempferol and isorhamnetin) were screened as xanthine oxidase inhibitors by ultrafiltration LC–MS, and the 50% scavenging concentration values of the screened flavonoids were lower than those for allopurinol. Lineweaver–Burk plot results indicated that kaempferol was a competitive xanthine oxidase inhibitor; the other flavonoids were all anticompetitive inhibitors. Four flavonoids—rutin, quercetin, kaempferol and isorhamnetin—were screened as superoxide anion radical scavengers by LC–MS. The results demonstrate that the method for screening and evaluation of superoxide anion radical scavenger and xanthine oxidase inhibitor from a complex mixture system is feasible and efficient.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2020
·Vol. 34
·期 7
·e4834
·
IF 1.728
Xiaoyue Shan,Siwei Tan,Yanpeng Shi,Ji Shao,Kewen Su,Ling Zhang,Hui Feng,Haipeng Ye
In this study, activated carbon/diatomite-based magnetic nancomposites (denoted as AC/DBMNs) were synthesized and applied as an adsorbent for magnetic solid-phase extraction of S- phenylmercapturic acid ( S- PMA) from human urine prior to high-performance liquid chromatography. The surface morphologies and structures of AC/DBMNs were characterized by Fourier transform infrared spectroscopy, transmission and scanning electron microscopy, X-ray diffraction, Brunauer–Emmett–Teller surface area, vibrating sample magnetometer and ζ -potential measurements. The experimental parameters including sample volume, sample pH, adsorbent amount, extraction time, elution solvent and desorption time were investigated in detail. Under the optimum conditions, the method exhibited good linearity ( r > 0.9993) within the concentration ranges of 0.03–1.0 mg/L. Moreover, the limits of detection and quantification were 0.01 and 0.03 mg/L, respectively. The enrichment factor was 5, and good recoveries (88.9–97.3%) with relative standard deviations in the range of 5.6–6.8% ( n = 6) for inter-day and 6.3–8.1% ( n = 6) for intra-day were achieved. The developed method was successfully applied to the analysis of S- PMA in urine samples. In addition, this accurate and sensitive method has great potential to be applied in the early screening and clinical diagnosis of the workers exposed to benzene.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2020
·Vol. 34
·期 7
·e4838
·
IF 1.728
De-en Han,Yanmei Shi,Ping Tian,Hengchao Wei,Mingsan Miao,Xiu-min Li
A rapid and sensitive method was developed and validated for the quantitative determination of xanthopurpurin (XPP) in rat plasma using ultra-performance liquid chromatography-electrospray ionization-Orbitrap mass spectrometry. XPP inhibits IgE production and prevents peanut-induced anaphylaxis. The XPP and emodin (internal standard) were determined in negative ion mode with m/z 239.0350 → 211.0400 and 269.0455 → 241.0507, respectively. The separation process was achieved using an ACQUITY UPLC HSS T 3 column with acetonitrile and 0.1% formic acid in water (85:15). The linear range was 0.5–100 ng/mL, and the correlation coefficient ( r 2 ) was > 0.993. The inter-day and intra-day precision was within an acceptable range of 15%. The extraction recovery and matrix effect were 78.9–87.2% and 94.3–98.5%, respectively. Under different conditions, the XPP was stable in the range of 5.6–10.6%. This method was successfully applied to study the pharmacokinetics of XPP with an oral dose of 10.0 mg/kg and intravenous dose of 2.0 mg/kg in rats. The absolute oral bioavailability of XPP was 4.6%.
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2020
·Vol. 34
·期 6
·e4824
·
IF 1.728
Chu Chu,Linmin Lian,Caijing Liu,Jing Li,Hui Mao,Luyi Jiang,Jizhong Yan
Electrokinetic supercharging, a convenient and powerful online preconcentration technique in capillary electrophoresis, was introduced and evaluated for the determination of two alkaloids, berberine and jatrorrhizine, in mice fecal samples for the first time. The method depended on using a bare fused silica capillary (50 cm × 50 μm i.d.) and applying the voltage of 25 kV with UV detection at 205 nm. Parameters that affect the separation and preconcentration efficiency have been optimized. The optimum conditions used were as follows: background electrolyte consisting of 40mM sodium dihydrogenphosphate containing 30% methanol (v/v); hydrodynamic injection of 20mM KCl (50 mbar × 150 s) as the leading electrolyte; electrokinetic injection of the sample (+15 kV, 120 s) followed by the hydrodynamic injection of 30mM dodecyl trimethyl ammonium chloride (50 mbar × 12 s) as the terminating electrolyte. The results showed that the detection sensitivity of berberine and jatrorrhizine was, respectively, improved up 2740- and 2928-fold compared with normal injection, providing limits of detection lower than 3 ng/mL with good repeatability in areas (relative standard deviation < 3%). In summary, the developed method proved its ability in analyzing trace alkaloids in complicated biological samples.
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