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Pharmacokinetics of tectorigenin, tectoridi, irigenin, and iridin in mouse blood after intravenous administration by UPLC-MS/MS

Li Jianbo, Yao Yuqi, Zhou Minyue, Yu Zheng, Jin Yinan, Wang Xianqin

Acta Chromatographica

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2022

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Vol. 34, no. 3

246--252

EN

Tectorigenin, tectoridin, irigenin, and iridin are the four most predominant compounds present in She Gan. She Gan has been used in traditional Chinese medicine because of its anti-inflammatory, hep- atoprotective, anti-tumor, antioxidant, phytoestrogen-like properties. In this paper, a UPLC-MS/MS method was developed to measure the pharmacokinetics of tectorigenin, tectoridin, irigenin, iridin after intravenous administration in mice. A UPLC BEH C18 (50 mm × 2.1 mm, 1.7 µm particle size) chromatographic column was utilized for separation of the four target analytes and internal standard (IS), and the analysis of blood plasma samples; the mobile phase consisted of an acetonitrile-water (w/0.1% formic acid) gradient elution. Electron spray ionization (ESI) positive-ion mode and multiple reaction monitoring (MRM) mode was used for quantitative analysis of the analytes and internal standard. The four compounds were administered intravenously (sublingual) at doses of 5 mg/kg. After blood sam- pling, samples were processed and then analyzed by UPLC-MS/MS. The linearity of the method was robust over the concentration range of 2-5,000 ng/mL. The intra-day precision of the analysis was within 15%, the inter-day precision was within 12%, and the accuracy was between 92% and 110%. The recoveries were 65–68%, and the matrix effect was 93-109%. The established UPLC-MS/MS detection method was then successfully applied to study the pharmacokinetics of tectorigenin, tectoridin, irigenin, iridin in mice.

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Determination of oroxin A, oroxin B, oroxylin A, oroxyloside, chrysin, chrysin 7-O-beta-gentiobioside, and guaijaverin in mouse blood by UPLC-MS/MS and its application to pharmacokinetics

Yu Zheng, Chen Fan, Jin Yinan, Zhou Minyue, Wang Xianqin, Shen Xiuwei

Acta Chromatographica

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2022

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Vol. 34, no. 4

394--402

EN

In this study, a UPLC-MS/MS method was developed to measure the concentrations of the flavonoids oroxin A, oroxin B, oroxylin A, oroxyloside, chrysin, chrysin 7-O-beta-gentiobioside, and guaijaverin in the blank mouse blood, and the method was then used in the measurement of the pharmacokinetics of the compounds in mice. Oroxin A, oroxin B, oroxylin A, oroxyloside, chrysin, chrysin 7-O-beta-gentiobioside, and guaijaverin were administered intravenously at a dose of 5 mg kg⁻¹, and the mouse blood (20 μL) was withdrawn from the caudal vein 0.08333, 0.25, 0.5, 1, 2, 4, 6, 8, and 10 h after administration. The mobile phase used for chromatographic separation by gradient elution was composed of acetonitrile and water (0.1% formic acid). The analytes were detected by operating in electrospray ionization (ESI) positive-ion mode using multiple reactions monitoring (MRM). The intra-day and inter-day accuracy ranged from 86.2 to 109.3%, the intra-day precision was less than 14%, and the inter-day precision was less than 15%. The matrix effect ranged from 85.3 to 111.3%, and the recovery of the analytes after protein precipitation were all above 78.2%. This method had the advantages of high sensitivity, accuracy, and recovery, and it had excellent selectivity, which enabled it to be applied to measuring the pharmacokinetics of the analytes in mice.

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Determination and pharmacokinetics of calycanthine in rat plasma by UPLC-MS/MS

Lu Meifei, Lu Xiaojie, Yu Zheng, Wen Congcong

Acta Chromatographica

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2021

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Vol. 33, no. 1

91--95

EN

Calycanthine is an important class of alkaloids extracted and isolated from the roots, leaves, flowers and fruits of Chimonanthus praecox. In this work, the UPLC-MS/MS method was used for determination of calycanthine in rat plasma, and the pharmacokinetics in rats were investigated. Midazolam was used as an internal standard (IS), and methanol precipitation method was used to pretreatment the rat plasma samples. Chromatographic separation was achieved on a UPLC BEH C18 (50 3 2.1 mm, 1.7 mm) column with the mobile phase of methanol- 0.1% formic acid aqueous solution with gradient elution. Multiple reaction monitoring (MRM) mode with positive ionization was applied for quantitative analysis, m/z 347.3 → 246.7 and 326.2 → 291.4 for calycanthine and IS, respectively. The results indicated that within the range of 1–200 ng/mL, linearity of calycanthine in rat plasma was good (r > 0.995), and the lower limit of quantification (LLOQ) was 1 ng/mL. Accuracy range was between 90.6 and 109.4%, precision (RSD) of calycanthine was less than 14%. The matrix effect was between 97.9% and 105.4%, the recovery was better than 85.6%. The developed UPLC-MS/MS method was successfully applied in the pharmacokinetics of calycanthine in rats after oral and intravenous administration. The absolute bioavailability of the calycanthine was 37.5% in rats.

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Determination of diosmetin-7-o-β-d-glucoside in rat plasma by UPLC–MS/MS

Li Jianbo, Yu Zheng, Han Cheng, Wang Zhening, Hu Yujie, Wen Congcong, Lin Chongliang

Acta Chromatographica

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2020

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Vol. 32, no. 4

264--268

EN

In this study, we used UPLC–MS/MS to determine diosmetin-7-o-β-d-glucoside in rat plasma and investigated its pharmacokinetics in rats. Six rats were given diosmetin-7-o-β-d-glucoside (5 mg/kg) by intravenous (i.v.) administration. The blood (150 μL) was withdrawn from the caudal vein after administration. Diazepam was used as an internal standard (IS), and a one-step acetonitrile precipitation method was used to process the plasma samples. Chromatographic separation was achieved using a UPLC BEH C18 column using a mobile phase of acetonitrile–0.1% formic acid with gradient elution. Electrospray ionization (ESI) tandem mass spectrometry in multiple reaction monitoring (MRM) mode with positive ionization was applied, 463.1 → 301.0 for diosmetin-7-o-β-d-glucoside, m/z 285.1 → 193.0 for diazepam (IS). Intra-day and inter-day precision of diosmetin-7-o-β-d-glucoside in rat plasma were less than 14%. The method was successfully applied in the pharmacokinetics of diosmetin-7-o-β-d-glucoside in rats after intravenous administration. The t1/2 of diosmetin-7-o-β-d-glucoside is 1.4 ± 0.4 h, which indicates the quick elimination.

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Pharmacokinetics of 8-O-acetylharpagide in mouse blood by UPLC–MS/MS

Chen Shanjiang, Huang Miaoling, Yu Zheng, He Jiamin, Huang Binge, Wang Xianqin, Ma Jianshe, Wen Congcong

Acta Chromatographica

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2019

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Vol. 31, no. 3

183--188

EN

8-O-Acetylharpagide is the main active component of the herb Ajuga decumbens, which possesses anti-tumor, anti-virus, and anti-inflammation properties. In this study, ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) was used to measure the concentration of 8-O-acetylharpagide in mouse blood, with subsequent investigation of the pharmacokinetics of the drug after intravenous or oral administration. Shanzhiside methyl ester was used as an internal standard, and the acetonitrile precipitation method was used to process the blood samples. Chromatographic separation was achieved using an ultra-performance liquid chromatography ethylene-bridged hybrid (UPLC BEH) column (2.1 mm × 50 mm, 1.7 μm) with a gradient methanol–water mobile phase (containing 0.1% formic acid). The flow rate was 0.4 mL/min, and the elution time was 5.0 min. 8-O-Acetylharpagide was quantitatively measured using electrospray ionization (ESI) tandem mass spectrometry in multiple reaction monitoring (MRM) mode with positive ionization. The result indicated that, within the range of 5–500 ng/mL, the linearity of 8-O-acetylharpagide in mouse blood was satisfactory (r > 0.995), and the lower limit of quantification (LLOQ) was 5 ng/mL. Intra-day precision relative standard deviation (RSD) of 8-O-acetylharpagide in blood was lower than 9%, and the inter-day precision RSD was lower than 13%. The accuracy range was between 94.3% and 107.1%, average recovery was higher than 91.3%, and the matrix effect was between 100.8% and 110.8%. This analytical method was sensitive and fast with good selectivity and was successfully applied to perform pharmacokinetic studies of 8-O-acetylharpagide in mice. The bioavailability of 8-O-acetylharpagide was 10.8%, and the analysis of the primary pharmacokinetic parameters after oral and intravenous administration indicated that 8-O-acetylharpagide had a significant first pass effect after oral administration.

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Determination of licochalcone A in rat plasma by UPLC–MS/MS and its pharmacokinetics

Weng Qinghua, Chen Lianguo, Ye Luxin, Lu Xiaojie, Yu Zheng, Wen Congcong, Chen R., Huang Gang

Acta Chromatographica

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2019

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Vol. 31, no. 4

262--265

EN

The aim of this study was to establish a rapid, sensitive, and selective ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method to quantify the concentrations of licochalcone A and applicate the technique to its pharmacokinetic study. Analytes were separated on an UPLC ethylene bridged hybrid (BEH) C18 column (2.1 mm × 50 mm, 1.7 μm). The mobile phase was consisted of acetontrile and 0.1% formic acid with a flow rate of 0.4 mL/min in a gradient elution mode. Multiple-reaction monitoring (MRM) was carried out in a negative mode for licochalcone A (m/z 337.2 → 119.7) and the internal standard (IS) (m/z 609.0 → 300.9). The linearity of licochalcone A was great from 0.53 to 530 ng/mL. The lower limit of quantification and the lower limit of detection were 0.53 ng/mL and 0.26 ng/mL, respectively. The intra-day precision was less than 14%, and the inter-day precision was no more than 11%. The accuracy was from 91.5% to 113.9%, the recovery was over 90.5%, and the matrix effect was between 84.5% and 89.7%. The results of stability were in an acceptable range. The bioavailability was only 3.3%, exhibiting poor absorption. The developed method was successfully applicable for determining the concentrations of licochalcone A and its pharmacokinetic study.