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Simultaneous determination of three active flavonoids in rat plasma by HPLC-MS/MS : application to a comparative pharmacokinetic investigation after oral administration of Schizonepeta tenuifolia aqueous extract with and without its volatile oil

Liu Siting, Jiang Yulan, Shan Mingqiu, Yu Sheng, Cheng Fangfang, Chen Peidong, Bao Beihua, Cao Yudan, Zhang Li, Wu Qinan

Acta Chromatographica

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2022

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Vol. 34, no. 1

32--40

EN

Schizonepeta tenuifolia Briq. (ST) has been used as an aromatic exterior-releasing medicine in clinical practice for thousands of years in China. Previous researches have revealed both volatile oil (STVO) and aqueous extract (STAE) from ST showed significant pharmacological activities, such as anti-virus, anti-inflammation, anti-oxidation, and immunoregulation. However, the influence between each other was still unknown. The purpose of this study was to compare the pharmacokinetic profiles of three main flavonoids (luteoloside, apigetrin, and hesperidin) in STAE to illustrate the influence of STVO. A liquid chromatography-tandem mass spectrometry (HPLC-MS) method was established to quantitatively analyze the three absorbed ingredients in the plasma of healthy rats. Biological samples were analyzed on an Agilent Eclipse Plus C18 column (3.0 mm × 150 mm, 3.5 μm) with gradient mobile phase (containing 0.2% formic acid and acetonitrile) at a flow rate of 0.8 mL/min. All the analytes and quercitrin (IS) were investigated with an electrospray ionization source (ESI) using multiple-reaction monitoring (MRM) in negative ionization mode. In addition, this quantitative method showed good linearities (r ≥ 0.9995) and the lower limits of quantification were 0.590–1.19 ng/mL. The intra- and inter-day precisions ranged 3.47–10.45% and 4.29–11.28% for the three analytes. The mean extraction recoveries were in the range of 77.41–109.79% and the average matrix effects were within 83.41–112.67%. The validated method has been fully applied to compare the pharmacokinetic parameters of the three flavonoid glycosides in rat plasma after oral administration of STAE and STAE+STVO. In comparison of luteoloside, apigetrin, and hesperidin in STAE group, it was found that different degree of increasing existed for the time to reach the maximum concentration (T max), elimination half-life time (T 1/2), the area under the concentration curves (AUC0→t and AUC0→∞) and the maximum concentrations (C max) in STAE+STVO group. As can be seen from above results, STVO could improve the absorption and bioavailability of the three analytes. These findings would provide some active and strong basis of safe clinical application for ST and further exploitation for STVO from the perspective of drug–drug interaction.

2

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

Han Jianwei, Zhu Wenbo, Yu Ling, Chen Yajun, Wu Gaosong, Wang Zhibin

Acta Chromatographica

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2022

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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

Pharmacokinetic analysis of atractylenolide III in rat plasma after oral administration of Atractylodes japonica rhizome extract by ultra-performance liquid chromatography-ion trap mass spectrometry

Kim Jung-Hoon

Acta Chromatographica

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2019

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Vol. 31, no. 4

266--271

EN

Atractylenolide III is one of the major bioactive compounds in Atractylodes japonica rhizome; it has been used clinically for the treatment of gastrointestinal disorders. In the present study, a simple, rapid, and selective analytical method was developed and validated for the quantification of atractylenolide III in rat plasma samples using ultra-performance liquid chromatography–ion trap mass spectrometry (UPLC–ion trap MS). Liquid–liquid extraction with ethyl acetate was used for plasma sample preparation. Bergapten was used as an internal standard (IS). The separation of compounds was carried out on a C18 column, with isocratic elution of 0.1% formic acid in water–acetonitrile (45:55, v/v) at 35 °C. Mass detection was performed in the positive ion mode, under optimized conditions for an electrospray ionization source at m/z 249.1 for atractylenolide III and m/z 217.0 for the IS. The methods of instrumental analysis and plasma sample extraction were validated in terms of precision, accuracy, matrix effect, and extraction recovery, with acceptable values. The present method was successfully applied to the pharmacokinetic study of atractylenolide III in rat plasma samples after oral administration of A. japonica rhizome extract.

4

Identification of multiple constituents in shuganjieyu capsule and rat plasma after oral administration by ultra-performance liquid chromatography coupled with electrospray ionization and ion trap mass spectrometry

Xiao Y. C., Liu L. T., Bian J. J., Yan C. Q., Ye L., Zhao M. X., Huang Q. S., Wang W., Liang K., Shi Z. F., Ke X.

Acta Chromatographica

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2018

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Vol. 30, no. 2

95--102

EN

Shuganjieyu (SGJY) capsule is a classical formula widely used in Chinese clinical application. In this paper, an ultra-performance liquid chromatography coupled with electrospray ionization and ion trap mass spectrometry has been established to separate and identify the chemical constituents of SGJY and the multiple constituents of SGJY in rats. The chromatographic separation was performed on a C18 RRHD column (150 × 2.1 mm, 1.8 μm), while 0.1% formic acid–water and 0.1% formic acid–acetonitrile was used as mobile phase. Mass spectral data were acquired in both positive and negative modes. On the basis of the characteristic retention time (Rt) and mass spectral data with those of reference standards and relevant references, 73 constituents from the SGJY and 15 ingredients including 10 original constituents and 5 metabolites from the rat plasma after oral administration of SGJY were identified or tentatively characterized. This study provided helpful chemical information for further pharmacology and active mechanism research on SGJY.

5

Development and validation of UPLC–MS/MS method for determination of eupatilin in rat plasma and its application in a pharmacokinetics study

Geng P., Luo X., Peng X., Lin Z., Chen W., Zhang J., Wen C., Hu L., Hu S.

Acta Chromatographica

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2018

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Vol. 30, no. 4

231--235

EN

Eupatilin, mainly derived from Artemisia asiatica (Asteraceae), is an O-methylated flavone with various bioactivities. In the present study, a validated ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was established for the quantification of eupatilin in rat plasma with the internal standard (IS) of tussilagone and the protein precipitation of plasma samples was performed using acetonitrile–methanol (9:1, v/v). The eupatilin and IS were eluted separately on a UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 μm) with the gradient mobile phase consisted of 0.1% formic acid and acetonitrile. The protonated analytes were quantified by multiple reactions monitoring (MRM) mode with an electrospray ionization (ESI) source operated in positive ion mode. The calibration plots were found to be linear over the range from 2 to 1000 ng/mL for eupatilin in rat plasma. Both of the intra-day and inter-day precision variations (RSDs) were ≤13%. The recoveries of eupatilin in rat plasma were between 83.7% and 94.6%, and the accuracy of the method ranged from 95.8% to 107.6%. In addition, the validated method was applied to pharmacokinetic study of eupatilin after an intravenous dose of 2 mg/kg to rats.

6

Liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the determination of Vildagliptin in rat plasma

Sakthimanigandan K., Ganesh M., Kanthikiran V., Sivakumar T., Jang H.

Acta Chromatographica

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2015

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Vol. 27, no. 2

295--307

EN

A new sensitive and validated liquid chromatography electro spray ion-tandem mass spectrometry (HPLC-ESI-MS/MS) method for the quantification of Vildagliptin (VG) in rat plasma has been developed and validated using repaglinide (RG) as an internal standard (IS). The analytes were extracted by liquid-liquid extraction using ethyl acetate. Elution of the VG and IS was achieved on a reverse phase Betasil (C18 50 mm 4.6 mm ID, 5 μ) column with an isocratic mobile phase composed of acetonitrile: 2 mM ammonium acetate (90:10 v/v). The analytes monitored in the Multiple Reaction Monitoring (MRM) mode were m/z 304.2→154.0 and 453.3→230.3 for VG and RG, respectively. The calibration curve was linear in the range of 1.57–501.21 ng/mL for VG with lower limit of quantification 1.57 ng/mL. The intra run and inter run precision values are within 11.70% for VG at LOQ level.

7

Gradient elution LC-MS determination of dasatinib in rat plasma and its pharmacokinetic study

Wen C, Zhang Q., He Y., Deng M, Wang X., Ma J.

Acta Chromatographica

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2015

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Vol. 27, no. 1

81--91

EN

A sensitive and simple liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) method for determination of dasatinib in rat plasma using one-step protein precipitation was developed. After addition of carbamazepine as internal standard (IS), protein precipitation by acetonitrile was used as sample preparation. Chromatographic separation was achieved on an SB-C18 (2.1 mm × 150 mm, 5 μm) column with methanol-0.1% formic acid as mobile phase with gradient elution. Electrospray ionization (ESI) source was applied and operated in positive ion mode; selective ion monitoring (SIM) mode was used to quantification using target fragment ions m/z 488.2 for dasatinib and m/z 338.7 for the IS. Calibration plots were linear over the range of 10–1000 ng mL−1 for dasatinib in rat plasma. Lower limit of quantification (LLOQ) for dasatinib was 10 ng mL−1. Mean recovery of dasatinib from plasma was in the range 82.2%–93.6%. Relative standard deviation (RSD) of intra-day and inter-day precision were both less than 8%. This developed method is successfully used in pharmacokinetic study of dasatinib in rats.

8

Development and validation of a gradient elution high-performance liquid chromatographic method for determination of talinolol in rat plasma: Application to a preclinical food-drug interaction study

Mahgoub H, Hanafy A., Bamane F. H., Radwan A. E.

Acta Chromatographica

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2015

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Vol. 27, no. 1

67--79

EN

A sensitive and reproducible high-performance liquid chromatographic (HPLC) method for determination of talinolol (TAL) in rat plasma was developed and validated using pindolol (PIN) as an internal standard. Both TAL and PIN were separated on a Zorbax Eclipse XDB C18 column by gradient elution with 0.1% aqueous formic acid and acetonitrile as the mobile phase. Detection was performed using fluorescence measurement at λex 249 nm and λem 333 nm. The method was validated and found to be linear in the range of 10–2000 ng mL−1. The limit of quantification was 10 ng mL−1 based on 100 μL of plasma. The variations for intra- and inter-day precision were less than 10%, and the accuracy values were between 92% and 102.9%. The extraction recoveries were more than 82%. The assay was successfully applied to an in-vivo pharmacokinetic study of TAL in rats that were administered a single oral dose of 10 mg kg−1 TAL. The maximum concentration (Cmax) and the area under the plasma concentration-time curve (AUC0–12) were 0.369 ± 0.024 μg mL−1 and 1.429 ± 0.027 μg h mL−1, respectively. The modulatory effect of apricot juice on P-glycoprotein-related efflux carriers was also investigated. Co-administration of apricot juice resulted in a significant increase of the amount of TAL in plasma (Cmax and AUC0–12 were 0.679 ± 0.021 and 2.357 ± 0.079, respectively; p < 0.05).

9

A Simple Liquid Chromatographic Method for the Determination of Tenofovir in Rat Plasma and Its Application to Pharmacokinetic Studies

Ravi P. R., Joseph S., Avula U. S. R., Anthireddy S.

Acta Chromatographica

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2015

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Vol. 27, no. 4

597--612

EN

The objective of this study was to develop and validate a novel, simple, and selective high-performance liquid chromatographic (HPLC) method with photodiode array detector for the estimation of tenofovir in rat plasma, which can be utilized in analyzing the pharmacokinetic samples from rats. Prior to analysis, an optimized protein precipitation technique was used to extract tenofovir from plasma. The mobile phase for this method comprised of 10 mM ammonium acetate buffer (pH 4) and methanol in the ratio of 97:3 υ/υ. Chromatographic separation of tenofovir was achieved using Spincotech C-18G enabled column (250 × 4.6 mm, 5 μm). Tenofovir was monitored at a wavelength of 260 nm, and the calibration curve was linear in the range of 250–4000 ng mL−1 (R2 = 0.999). High recovery obtained after extraction (97%–101%) of plasma samples precluded the use of an internal standard. Validation studies were performed as per the standard guidelines, and the developed method was accurate, precise, and selective for the determination of tenofovir in the rat plasma. The stability studies performed during the sample pretreatment process and sample storage conditions did not show a quantifiable degradation of tenofovir. Further, this method was able to estimate tenofovir and determine its pharmacokinetic parameters, post IV bolus administration in male Wistar rats. The pharmacokinetic profile of tenofovir followed one compartmental open model.

10

Using LC-MS/MS to study dauricine pharmacokinetics and determine its bioavailability following administration in different routes

Gao X., Jiang X., Wang L.

Acta Chromatographica

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2013

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Vol. 25, no. 2

241--256

EN

Dauricine has a variety of pharmacological properties including anti-inflammatory, anti-arrhythmic, and antihypertensive effects as well as reversing multidrug resistance (MDR) of cancer cells. While its therapeutic application is increasing, its bioavailability of different administration routes has not been studied. In the present study, we developed and validated a liquid chromatography/electrospray ionization mass spectrometry method (LC-MS/MS). Using this method, we quantified dauricine in rat plasma after administration via intravenous (i.v.) injection, per oral (p.o.), and intraperitoneal injection (i.p.). Our results indicated that this method detected plasma dauricine with a good linearity in the range of 1.95–1000.00 ng/mL (r = 0.9997). The extraction method showed an average intra- and inter-day recovery of 98.21–104.35% and 98.0–103.58%, respectively. Dauricine showed a fast absorption and widespread distribution after administration in all three tested routes. After intravenous administration (2.5, 5.0, 10.0 mg/kg), the pharmacokinetics of dauricine exhibited a first-order kinetics. In addition, dauricine showed a slow elimination with a long half-life (t1/2z) and double peaks phenomenon following p.o. and i.p. administration. Furthermore, using area under the plasma concentration-time curve (AUC), we calculated absolute bioavailability, which was over twofold higher when administered via i.p. than via p.o. administration. The newly obtained information from our study will provide important reference for dauricine dose and administration route in designing dauricine therapy for applicable diseases.