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1

Development and validation of a rapid UHPLCMS/MS method for the determination of fenofibric acid in human plasma: application to a pharmacokinetic study of fenofibrate tablet in Chinese subjects

100%

Wu X. , Wang Y. , Liang B. , Wu H. , Wu L. , Song J. , Liu J.

Acta Chromatographica

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2021

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tom Vol. 33, no. 4

309--314

EN

An ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS) method was developed to determine the fenofibric acid (FA) in human plasma and applied to a pharmacokinetic study of fenofibrate tablet (Lipanthyl® supra, 160 mg) on Chinese subjects which had not been reported. Bezafibrate was used as an internal standard (IS), and the plasma samples were precipitated by methanol. Multiple reaction monitoring (MRM) mode was used to quantitatively analyzed FA m/z 317.2→230.7 and the IS m/z 360.0→274.0 in the electrospray ionization (ESI) negative interface. The calibration curves were linear over the range of 50–30,000 ng/mL (r2 ≥ 0.996). The intra-day and interday precision (coefficient of variation, CV%) was less than 2.7 and 2.5%, respectively. The accuracy (relative error, RE%) ranged from 4.5 to 6.9%. The average recovery was higher than 86.2%, and the matrix effect was between 95.32 and 110.55%. The simple, rapid, and selectivity method was successfully applied to the pharmacokinetic study of fenofibrate tablets on Chinese subjects.

2

Simultaneous determination and pharmacokinetics studies of five isoflavones in rat plasma by UHPLC-MS/MS after oral administration of Radix Astragali extract

88%

Han J. , Zhu W. , Yu L. , Chen Y. , Wu G. , Wang Z.

Acta Chromatographica

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2022

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tom Vol. 34, no. 1

24--31

EN

A rapid, sensitive and convenient method based on ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) was developed and validated for the simultaneous quantification of calycosin-7-O-β-d-glucoside (CCSG), ononin, calycosin, (6aR,11aR)-9,10-dimethoxypterocarpan-3-O-β-d-glucopyanoside (DPPG), and 7,2′-dihydroxy-3′,4′-dimethoxyisoflavan-7-O-β-d-glucopyanoside (DIFG) in rat plasma after oral administration of the methanol extraction from Radix Astragali. Theophylline played the role of internal standard (IS). Preparation of plasma samples by liquid-liquid extraction method with ethyl acetate after precipitation of protein with methanol. The analytes were detected with a triple quadrupole tandem mass spectrometery (MS) in multiple reaction monitoring (MRM) mode and a positive ion electrospray ionization (ESI). The method was validated with the concentration ranges of 1.96–62.69 ng/mL for CCSG, 1.70–54.5 ng/mL for ononin, 1.85–59.06 ng/mL for calycosin, 2.14–137.24 ng/mL for DPPG and1.96–125.25 ng/mL for DIFG, respectively. The method had the lower limit of quantification (LLOQ) with 0.49, 0.21, 0.92, 1.07, and 0.98 ng/mL for CCSG, ononin, calycosin, DPPG and DIFG respectively, and the precision less than 10%. The RSD of the accuracy was in the range of −4.35–8.91%. The results may be helpful to provide more accurate references to clinical application of this herb.

3

Validation and quantification of a UPLC-MS/MS method for the simultaneous determination of quinocetone and its main metabolites (3-methylquinoxaline-2-carboxylic acid and dedioxoquinenone) in aquatic products

88%

Tian X. , Han D. , Cui Y. , Ren L. , Jiang F. , Huang H. , Gong X. , Xue J. , Li J. , Liu H. , Xu Y. , Luo X. , Liu X. , Zhang X.

Acta Chromatographica

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2022

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tom Vol. 34, no. 4

444--452

EN

A sensitive and validated method for determining quinocetone and its main metabolites (3-methylquinoxaline-2-carboxylic acid and dedioxoquinenone) was established in aquatic products using ultra-high-performance liquid chromatography-tandem spectrometry (UHPLC-MS/MS). Samples were extracted with 2.0 mol L⁻¹ hydrochloric acid, then purified on MAX columns. After extraction and purification, the supernatant was evaporated to dry nearly under a gentle stream of nitrogen at 40 °C. Formic acid-acetonitrile-water (0.1/30/70, v/v/v) was adjusted to 1.00 mL final volume. An aliquot (10 μL) was injected into the C18 column for separation with the mobile phase of acetonitrile and 0.5% formic acid in water at 0.25 mL min⁻¹. Calibration curves were linear ranged from 10.00 ng mL⁻¹ to 200.0 ng mL⁻¹ for quinocetone and 3-methylquinoxaline-2-carboxylic acid, and 20.00 ng mL⁻¹ to 400.0 ng mL⁻¹ for dedioxoquinenone. Mean recoveries were 70%–89%, 73%–83% and 72%–84%, respectively. The limit of detection (LOD) was 1.00 μg kg⁻¹, 1.00 μg kg⁻¹ and 2.00 μg kg⁻¹, and quantification (LOQ) were 2.00 μg kg⁻¹, 2.00 μg kg⁻¹ and 4.00 μg kg⁻¹ for quinocetone, 3-methylquinoxaline-2-carboxylic acid, and dedioxoquinenone. Based on the method above, the analytes were determined in Apostichopus japonicus, three fishes (including Ctenopharyngodon idellus, Crucian carp and Oreochromis mossambicus), Penaeus vannamei, Penaeus chinensis, and Chlamys farreri. The method shows good sensitivity, linearity, precision, and accuracy. In short, the proposed method was reliable for the determination of quinocetone, 3-methylquinoxaline-2-carboxylic acid, and dedioxoquinenone in aquatic products.

4

Optimized ultra-high-performance liquid chromatography tandem mass spectrometry method for detecting compositional changes in Eucommia ulmoides and Achyranthes bidentata paired decoctions in vitro and in vivo

75%

Chen C. , Lv L. , Huang Y. , Gao M. , Jiang X. , Ge X. , Zheng D. , Bao L.

Acta Chromatographica

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2024

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tom Vol. 36, no. 1

31--44

EN

Rationale: The bark of Eucommia ulmoides and the roots of Achyranthes bidentata are commonly used in traditional Chinese medicine, and their pairing appears in many traditional Chinese medicine formulas as a recognized compatible unit. However, the changes and interactions of the main components of these two formulas when paired remain unclear, and there is currently no standard or method for their quality control and assessment of pharmacological effects. Methods: An optimized ultra-high-performance liquid chromatography triple-quadrupole mass spectrometry (UHPLC-MS/MS) method was established for the simultaneous identification of 10 components in E. ulmoides and A. bidentata using in vitro and in vivo models. Tributyltin methacrylate was the internal standard solution, and the blood samples were treated by an organic solvent precipitation method. Gradient elution was conducted on a C₁₈ column at 25 °C with 0.1% formic acid water:acetonitrile as the mobile phase at a flow rate of 0.5 mL min⁻¹. Dynamic multiple response monitoring was performed in negative-ion mode using an Agilent Jet Stream electrospray ionization ion source. Results: In negative-ion detection mode, eucommiol exhibited a good response, and the isomers ginsenoside Ro and achyranthoside C could also be well separated. The developed method accurately detected the five components with a low blood content. Compared to controls, the levels of ginsenoside Ro, chikusetsusaponin Ⅳa, and achyranthoside C increased; the contents of geniposidic acid and pinoresinol diglucoside were unchanged; and the levels of eucommiol, geniposide, β-ecdysterone, genipin, and achyranthoside D decreased in vitro. In vivo, the contents of geniposidic acid, geniposide, pinoresinol diglucoside, and β-ecdysterone were reduced; the contents of eucommiol and ginsenoside Ro were unchanged; and those of achyranthoside D, chikusetsusaponin Ⅳa, and achyranthoside C increased compared to the corresponding levels in the internal control. Conclusions: A method for the quality control of the E. ulmoides-A. bidentata drug pair was established for the first time and the main components in 10 drug pairs could be determined simultaneously in vitro and in vivo. These findings show that the E. ulmoides and A. bidentata drug pair cause a compositional change, providing new ideas for the development of this combination to improve clinical efficacy.

5

Multiresidue determination of antibiotics in preserved eggs using a QuEChERS-based procedure by ultrahigh-performance liquid chromatography tandem mass spectrometry

75%

Li Y. , Chen Z. , Wen S. , Hou X. , Zhang R. , Ma M.

Acta Chromatographica

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2018

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tom Vol. 30, no. 1

9--16

EN

A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method and ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC–MS/MS) were optimized and validated for 16 antibiotics belonging to three families (macrolides, quinolones, and sulfonamides) that were found in preserved eggs. Samples were extracted in 4 mL water and 10 mL acetonitrile with 1% acetic acid and subjected to a cleanup procedure using dispersive solid-phase extraction with C18 and primary secondary amine sorbents, prior to detection by UHPLC–MS/MS. Matrix-matched calibration was used for quantification to reduce the matrix effect with limits of quantification in the range of 0.3–3.0 μg/kg. Validation of the method was conducted by recovery and precision experiments. Recoveries of the spiked samples ranged from 73.8% to 127.4%, and the intra- and inter-day relative standard deviations were lower than 21.2% and 22.3%, respectively. This method was successfully applied to the analysis of antibiotics in preserved egg samples.