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3 Acta Chromatographica

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Determination of modafinil in rat plasma by UPLC-MS/MS and a study of its pharmacokinetics and bioavailability

He Yan, Ma Yizhe, Luo Lvqi, Chen Junying, Wen Congcong, Zhang Meiling

Acta Chromatographica

2023

Vol. 35, no. 2

187--192

Modafinil has a strong and long-lasting awakening effect. Short-term use can improve cognitive and work efficiency. Therefore, it has been known to be abused by students and parents as a “smart drug.” It is in the first category of psychotropic drugs and strictly controlled. To detect modafinil in rat plasma and study the differences in the pharmacokinetics of modafinil between oral and sublingual administration in rats, an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed. Rats were injected with modafinil by oral gavage and sublingual vein, respectively, blood was collected within a certain period, and the plasma was obtained by centrifugation. Midazolam was used as the internal standard, and the concentration of modafinil in the plasma was determined by UPLC-MS/MS, where a drug-time curve was created to calculate the pharmacokinetic parameters. The standard curve for modafinil ranged from 1 to 2000 ng mL⁻¹ with good linearity. The intra-day accuracy of modafinil was between 86% and 104%, and the intra-day accuracy was between 90% and 103%. Intra-day precision (RSD%) was less than 15%, inter-day precision (RSD%) was less than 15%. The matrix effect was between 93% and 102%, and the recovery was greater than 91%. The UPLC-MS/MS method established in this work has good selectivity and high sensitivity, and the UPLC-MS/MS method was successfully applied to the pharmacokinetics of modafinil by oral gavage and sublingual injection in rats. The bioavailability of modafinil was calculated to be 55.8%.

An UPLC-MS/MS method for quantification of spiraeoside in mouse blood and its application to a pharmacokinetic and bioavailability study

Cai Xiaojun, Dai Xiangyi, Li Zhou, Chen Junying, Wang Xianqin, Zhang Meiling

Acta Chromatographica

2023

Vol. 35, no. 3

272--277

A simple, rapid, and sensitive method based on UPLC-MS/MS was developed to determine spiraeoside in mouse blood, and was applied to the pharmacokinetics and bioavailability of spiraeoside after mice after intravenous (a dose of 5 mg kg⁻¹) and oral (a dose of 20 mg kg⁻¹) administration. On HSS T3 column set at 40 °C, chromatographic separation was obtained with the mobile phase of acetonitrile and 0.1% formic acid using the gradient elution. Spiraeoside and internal standard (IS) were quantitatively analyzed using multiple reaction monitoring (MRM) mode in electrospray (ESI) positive interface. The MRM mode was monitoring the fragmentation of m/z 465.4→303.1 and m/z 451.3→ 289.2 for spironoside and IS, respectively. The results showed a good linear relationship was in the concentration range of 1–200 ng mL⁻¹ (r > 0.998) and the lower limit of quantification (LLOQ) was 1.0 ng mL⁻¹. The intra- and the inter-day precision (RSD%) of the method was within 14.0%, and the accuracy ranged from 90.0% to 115.0%. The extraction recovery of spriaeoside was better than 63.0%, and the matrix effects were in the range of 86%–98%. It also showed the half-life was short, and the absolute bioavailability was 4.0% in mice. Therefore, the established UPLC-MS/MS method was suitable for the pharmacokinetic and bioavailability study of spiraeoside in mice.

Determination and pharmacokinetics and bioavailability of O-demethyl nuciferine in mice by UPLC–MS/MS

Wu Haiya, Lu Mengrou, He Jiamin, Huang Miaoling, Zheng Aote, Zhang Meiling, Wen Congcong, Ye Jufen

Acta Chromatographica

2019

Vol. 31, no. 3

222--227

In this study, a precise, rapid, and accurate ultra-performance liquid chromatography–tandem mass spectrometer (UPLC–MS/MS) method for the quantitation of O-demethyl nuciferine in mouse blood was developed, and pharmacokinetics of O-demethyl nuciferine was studied for the first time after sublingual injection and gavage. The study was performed with an UPLC ethylene bridged hybrid (UPLC BEH) (2.1 mm × 50 mm, 1.7 μm) column at 30 °C, using diazepam as the internal standard (IS). The mobile phase consisted of acetonitrile–10 mmol/L ammonium acetate (containing 0.1% formic acid), with a flow rate of 0.4 mL/min for 4 min run time. Multiple reaction monitoring (MRM) modes of m/z 282.1→219.0 for O-demethyl nuciferine and m/z 296.2→265.1 for IS were utilized to conduct quantitative analysis. Protein in mouse blood was directly precipitated with acetonitrile for sample preparation. The linear range was 1–500 ng/mL with r > 0.995, and the lower limits of quantification (LLOQ) was 1 ng/mL. The intra- and inter-day precision of O-demethyl nuciferine in mouse blood were RSD < 14% and RSD < 15%, respectively.r The accuracy ranged from 89.0% to 110.7%, with a recovery higher than 88.9%, while the matrix effect was between 103.1% and 108.7%. We further applied this UPLC–MS/MS method to the pharmacokinetic study on O-demethyl nuciferine after sublingual injection and gavage and determined the bioavailability to be 6.4%.