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Validated UPLC-MS/MS method for the determination of ivosidenib in rat plasma: Application to a pharmacokinetic study

Chen Minle, Xu Jia, Chen Feifei, Zhou Quan, Wang Shuanghu, Han Aixia

Acta Chromatographica

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2023

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Vol. 35, no. 3

227--232

EN

Ivosidenib (AG-120) is an unlisted, but estimated to be valid, oral inhibitor for isocitrate dehydrogenase 1 (IDH1) in the phase Ⅰ study of IDH1-mutated acute myeloid leukemia (AML) patients. This paper presents the investigation and validation of a rapid, effective, qualitative and quantitative determination method of ivosidenib in rat plasma by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The samples were treated using acetonitrile precipitation to remove protein influence. Then, the supernatant was extracted to analyze plasma concentration traits. In the UPLC system, acetonitrile and water containing 0.1% formic acid were selected as a cosolvent mobile phase, applying a gradient elution to isolate compounds in a C18 column. Mass detections were performed on a triple quadruple mass spectrometer in positive ion mode. Electroshock characteristic fragment ionization was used for m/z 583.95→214.53 for ivosidenib for quantitative determination, m/z 583.95→186.6 for qualitative determination, and m/z 492.06→354.55 for IS. The selectivity, linearity, stability, accuracy and precision were verified by reaching the guideline criteria from European Medicine Agency (EMA) and the Food and Drug Administration (FDA). The calibration curve was linear over the concentration range of 2–2,000 ng mL⁻¹ for ivosidenib in rat plasma with a lower limit of quantification (LLOQ) of at least 2 ng mL⁻¹. Additionally, there was no distinct matrix effect or carry-over phenomenon. The method was successfully established and applied to separate ivosidenib from plasma, with the entire analytical process being performed within 3 min for each sample, which shows high-efficiency and convenience for further studies of ivosidenib.

2

Simultaneous determination of six triterpenoid saponins in beagle dog plasma by UPLC-MS/MS and its application to a pharmacokinetic study after oral administration of the extract of the Eleutherococcus senticosus (Rupr. & Maxim.) Maxim. leaves

Wang Zhibin, Chang Yaodan, Cao Feng, Yang Chunjuan, Wang Zhenyue, Kuang Haixue

Acta Chromatographica

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2023

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Vol. 35, no. 1

88--98

EN

A rapid and simple ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) method was developed and validated for simultaneous determination of six analytes from the Eleutherococcus senticosus (Rupr. & Maxim.) Maxim. leaves (ESL) in beagle dog plasma for the first time, including 3-O-α-ʟ-rhamnopyranosyl-(1→2)-α-ʟ-arabinopyranoside-29-hydroxy oleanolic acid, 3-O-β-ᴅ-glucopyranosyl-(1→2)-α-ʟ-arabinopyranoside-29-hydroxy oleanolic acid, 3-O-β-ᴅ-glucopyranosyl-(1→2)-α-ʟ-arabinopyranosyl-30-norlean-12,20 (29) –dien-28-olic acid, ciwujianoside E, guaianin N, and eleutheroside K. The chromatographic separation was performed using an ACQUITY UPLC BEH C18 column (2.1 × 100 mm, 1.7 μm) using a gradient elution way with a mobile phase of acetonitrile-water containing 0.1% formic acid. Analytes were detected on a triple-quadrupole mass spectrometer equipped with an electrospray ionization (ESI) source with multiple reaction monitoring (MRM) mode. Calibration curves were all linear (r ≥ 0.9933) over the concentration range. The mean extraction recoveries and matrix effect of analytes and I.S. were ranged from 80.26% to 98.32% and from 91.27% to 111.67%, respectively. The intra-day and inter-day precision were ranged from 2.20% to 14.81%, and the accuracy range was 1.60–14.60%. The analytical method was successfully applied for the pharmacokinetic characteristics of the six analytes in beagle plasma after oral administration of ESL extracts. The T1/2 of six analytes was more than 3.09 ± 0.78 h.

3

Pharmacokinetics and bioavailability of curdione in mice by UPLC-MS/MS

Liang Qishun, Chen Tianyu, Luo Lvqi, Ma Yizhe, Wen Congcong, Huang Xueli

Acta Chromatographica

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2023

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Vol. 35, no. 2

144--148

EN

A UPLC-MS/MS method was developed to determinate curdione in the mouse blood, and the pharmacokinetics of curdione in mice after intravenous (5 mg kg⁻¹) and oral (20 mg kg⁻¹) administration were studied. The HSS T3 column was used for separation, and column temperature was set at 40 °C. Multiple reaction monitoring (MRM) mode were used for determination of curdione. Blood samples were taken from the caudal vein of Institute of Cancer Research (ICR) mice after administration of curdione. It showed a good linear relationship in the range of 1–500 ng mL⁻¹ (r > 0.998); the intra-day precision was <13%, the inter-day precision was <15%, and the accuracy was 90%–105%, the recovery was >77%, and the matrix effect was 97%–107%. The half-life was relatively short, and the bioavailability was 6.5%. The developed method was suitable for the pharmacokinetics of curdione in mice.

4

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

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2023

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Vol. 35, no. 2

187--192

EN

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%.

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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

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2023

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Vol. 35, no. 3

272--277

EN

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.

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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.

7

Multi-pharmaceuticals analysis in fish by continuous series solid-phase extraction coupled with UPLC-MS/MS

Gao Lei, Wang Peng, Chen Zhongxiang, Tang Shizhan, Wu Song, Li Gang, Qin Dongli

Acta Chromatographica

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2022

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Vol. 34, no. 1

61--70

EN

Pharmaceuticals which are widely used in aquatic can easily migrate into the environment and aquatic animals, and can increase the risk of drug resistance and allergic symptoms if consumed by humans. In order to achieve high-throughput analysis of pharmaceuticals with different physical and chemical properties from complex matrices, we developed a new method for various types pharmaceuticals in fish and shrimp tissue. Series solid-phase extraction (s-SPE) with different adsorbents was selected for extracting and purifying analytes with different paddings. s-SPE were combined with ultra performance liquid chromatography triple quadruple tandem mass spectrometry (UPLC-MS/MS) for the detection of 30 pharmaceuticals antibiotics in fish samples. This method was stabilized and reliable to determinate the pharmaceuticals in fish and shrimp samples. As the method combined multiple Chinese national standards method, it could be easily treat the multi-pharmaceuticals from the fish and shrimp samples once time. It provided for both quantitative and qualitative methods and they could be applied to single- or multi-residue methods.

8

Development of a rapid UPLC-MS/MS method for the determination of toddalolactone in mouse blood and its application in pharmacokinetics

Zhou Jing, Wang Hongzhe, Miao Caiyun, Yao Yunxi, Ma Jianshe

Acta Chromatographica

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2022

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Vol. 34, no. 1

18--23

EN

A rapid and simple UPLC-MS/MS method was developed to determine toddalolactone in mouse blood and applied to measure the pharmacokinetics of toddalolactone in mice. Blood samples were first preprocessed by ethyl acetate liquid-liquid extraction. Oxypeucedanin hydrate (internal standard, IS) and toddalolactone were gradient eluted from a UPLC BEH C18 column using a mobile phase consisting of acetonitrile and water (0.1% formic acid). Using electrospray ionization (ESI) as the ionization source, multiple reaction monitoring was used to detect the precursor and product ions of m/z 309.2 and 205.2, respectively, for toddalolactone and of m/z 305.1 and 203.0 for IS, respectively, for quantitative detection. A calibration curve was run over the concentration range of 5–4,000 ng/mL (r > 0.995). The matrix effects ranged from 93.5 to 98.4%, and the recovery was higher than 77.3%. The precision was less than 13%, and the accuracy ranged from 90.9 to 108.4%. The developed UPLC-MS/MS method was successfully used for measuring the pharmacokinetics of toddalolactone in mice after oral (20 mg/kg) and intravenous administration (5 mg/kg), and the absolute bioavailability of toddalolactone was 22.4%.

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Development and validation of UPLC-MS/MS method for in vitro quantitative analysis of pyrazinamide in lipid core-shell nanoarchitectonics for improved metabolic stability

Thalla Maharshi, Jala Aishwarya, Borkar Roshan M., Banerjee Subham

Acta Chromatographica

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2022

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Vol. 34, no. 3

237--245

EN

Pyrazinamide (PZA), a medication for tuberculosis, has high aqueous solubility and low permeability, undergoes extensive liver metabolism, and exhibits liver toxicity through its metabolites. To avoid this, PZA in lipid core-shell nanoarchitectonics has been formulated to target lymphatic uptake and provide metabolic stability to the incorporated drug. The UPLC-MS/MS method for reliable in vitro quantitative analysis of pyrazinamide (PZA) in lipid core-shell nanoarchitectonics as per ICH guidance was developed and validated using the HILIC column. The developed UPLC-MS/MS method is a simple, precise, accurate, reproducible, and sensitive method for the estimation of PZA in PZA-loaded lipid core-shell nanoarchitectonics for the in vitro determination of % entrapment efficiency, % loading of pyrazinamide, and microsomal stability of lipid core-shell nanoarchitectonics in human liver micro- somes. The % entrapment efficiency was found to be 42.72% (±12.60). Lipid nanoarchitectonics was found to be stable in human liver microsomes, where %QH was found to be 6.20%, that is, low clearance. Thus, this formulation is suitable for preventing PZA-mediated extensive liver metabolism. These findings are relevant for the development of other lipid-mediated, suitable, stable nano- formulations containing PZA through various in vitro methods.

10

Determination of narciclasine in mouse blood by UPLC-MS/MS and its application to a pharmacokinetic study

Ren Ke, Feng Tiantian, Shi Hai, Ma Jianshe, Jin Yongxi

Acta Chromatographica

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2022

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Vol. 34, no. 2

115--119

EN

Narciclasine is a 7-hydroxy derivative of lycorisidine. It was the first alkaloid isolated from the stem of narcissus (Amaryllidaceae) in 1967. Six mice were given narciclasine (5 mg/kg) by intravenous administration. A UPLC-MS/MS method was developed to determine narciclasine in mouse blood. Tectorigenin (internal standard, IS) and narciclasine were gradient eluted by mobile phase of methanol and 0.1% formic acid in a BEH C18 column. The multiple reaction monitoring (MRM) of m/z 308.1→248.1 for narciclasine and m/z 301.1→286.0 for IS with an electrospray ionization (ESI) source was used for quantitative determination. The calibration curve ranged from 1 to 6,000 ng/mL. The accuracy was from 92.5 to 107.3%, and the matrix effect was between 103.6 and 107.4%. The developed UPLC-MS/MS method was successfully applicated to a pharmacokinetic study of narciclasine in mice after intravenous administration (5 mg/kg).

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Determination of eugenitin in mouse blood by ultra-performance liquid chromatography-tandem mass spectrometry and its application to a pharmacokinetic study

Lin Chongliang, Song Dezhen, Jiang Haodong, Luo Lvqi, Bao Xi, Yu Xiaomin, Ma Jianshe, Wang Xianqin, Jiang Xiajuan

Acta Chromatographica

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2022

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Vol. 34, no. 3

253--257

EN

Eugenitin is a non-volatile chromone derivative which is always found in dried flower buds of Syzygium aromaticum L. (Merr.) & L.M. Perry. Until now, there were no reports about the pharmacokinetics of eugenitin in biological fluids. A UPLC-MS/MS method developed to determine eugenitin in mouse blood. The blood samples were prepared by protein precipitation with acetonitrile. Chrysin (internal standard, IS) and eugenitin were gradient eluted by mobile phase of acetonitrile and water (0.1% formic acid) in a BEH C18 column. The multiple reaction monitoring (MRM) of m/z 221.1→206.0 for eugenitin and m/z 255.1→152.9 for IS with an electrospray ionization (ESI) source was used for quantitative detection. The calibration curve ranged from 0.5 to 500 ng/mL (r > 0.995). The accuracy ranged from 98 to 113%, the precision was less than 12%, and the matrix effect was between 86 and 94%, the recovery was better than 81%. The developed method was successfully used for pharmacokinetics of eugenitin in mice after intravenous (5 mg/kg) and oral (20 mg/kg) administration, and the absolute availability of eugenitin was 12%.

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Simultaneous determination of carbofuran and 3-hydroxycarbofuran in duck liver by an UPLCMS/MS

Chen Siyuan, Yu Yang, Ma Jianshe, Wen Congcong, Wang Xianqin, Zhou Quan

Acta Chromatographica

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2021

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Vol. 33, no. 4

354--360

EN

Carbofuran is a carbamate pesticide, a broad-spectrum, high-efficiency, low-residue, and highly toxic insecticide, acaricide, and nematicide, widely used in agriculture. Carbofuran is most harmful to birds, and birds or insects killed by furan poisoning can be killed by secondary poisoning after being foraged by raptors, small mammals, or reptiles. In this paper, an UPLC-MS/MS method was developed for the determination of carbofuran and its metabolite, 3-hydroxycarbofuran, in duck liver. Liver tissue was first ground into a homogenate and then passed through ethyl acetate liquid-liquid extraction processing samples. Multiple reaction monitoring (MRM) mode was used for quantitative analysis, m/z 222.1 → 165.1 for carbofuran, m/z 238.1 → 180.9 for 3-hydroxycarbofuran and m/z 290.2 → 198.2 for an internal standard. The standard curves of carbofuran and 3-hydroxycarbofuran in duck liver were within a range of 2–2000 ng/g, where the linearity was good, the lower limit of quantification was 2 ng/ g. The intra-day precision of carbofuran and 3-hydroxycarbofuran was <14%, and the inter-day precision was <13%, the accuracy range was between 91.8 and 108.9%, the average extraction efficiency was higher than 75.1% with a matrix effect between 93.4 and 107.7%. The developed method was applied to a situation of suspected duck poisoning at a local farm.

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Pharmacokinetics of palmatine in rat after oral and intravenous administration by UPLC-MS/MS

Li Jianbo, Hu Yujie, Wu Yajin, Feng Tiantian, Wen Congcong, Jiang Xiajuan

Acta Chromatographica

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2021

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Vol. 33, no. 1

25--29

EN

Palmatine is a compound with good water solubility extracted from Coptis chinensis, Fibraurea recisa Pierre, Cortex Phellodendri Chinensis. Palmatine has good antibacterial activity and mainly used for the treatment of bacterial dysentery, gynecological inflammation, surgical infection, and conjunctivitis. It has anti-diabetic, anti-oxidant, and cognitive-enhancing activities. In this study, we used UPLC-MS/MS to determinate palmatine in rat plasma, and investigated its pharmacokinetics. Coptisine was utilized as an internal standard (IS), and acetonitrile precipitation method was used to process the plasma samples. Chromatographic separation was achieved using a UPLC BEH C18 column using 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. The results indicated that within the range of 1–500 ng/mL, linearity of palmatine in rat plasma was acceptable (r > 0.995), and the lower limit of quantification (LLOQ) was 1 ng/mL. Intra-day and inter-day precision RSD of palmatine in rat plasma were less than 14%. Accuracy range was between 93.7 and 107.1%, and matrix effect was between 101.6 and 109.4%. The method was successfully applied in the pharmacokinetics of palmatine in rats after oral and intravenous administration. The absolute bioavailability of the palmatine was 15.5% in rats.

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Pharmacokinetics and bioavailability of liensinine in mouse blood by UPLC-MS/MS

Tong Shuhua, Zeng Yuqi, Ma Jianshe, Wen Congcong

Acta Chromatographica

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2021

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Vol. 33, no. 4

333--337

EN

Liensinine is a bisbenzyltetrahydroisoquinoline alkaloid extracted from lotus (Nelumbo nucifera GAERTNER., Nelumbonaceae), especially in its embryo loti “Lien Tze Hsin” (green embryo of mature seed). A rapid and simple UPLC-MS/MS method was developed to determine liensinine in mouse blood and its application to a pharmacokinetic study. The blood samples were preprocessed by protein precipitation using acetonitrile. Midazolam (internal standard, IS) and liensinine were gradient eluted by mobile phase of methanol and water (0.1% formic acid) in a Waters UPLC BEH C18 column. The multiple reaction monitoring of m/z 611.3 → 206.1 for liensinine and m/z 326.2 → 291.1 for IS with an electrospray ionization (ESI) source was used for quantitative detection. The calibration curve ranged from 0.5 to 400 ng/mL (r > 0.995). The accuracy ranged from 92.2 to 108.2%, the precision of intra-day and inter-day was less than 14%, and the matrix effect was between 100.0% and 109.6%, the recovery was better than 71.0%. The developed UPLC-MS/MS method was successfully used for a pharmacokinetic study of liensinine in mice after oral (5 mg/kg) and intravenous administration (1 mg/kg), and the absolute availability of liensinine was 1.8%.

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Effect of Citrus suavissima Hort. ex Tanaka on pharmacokinetics of erlotinib in rat plasma by UPLC-MS/MS

Yang Jinzhao, Liu Huamin, Cai Yuan, Wu Yazhen, Xu Xiaoxin, Wang Xianqin, Lin Chongliang

Acta Chromatographica

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2021

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Vol. 33, no. 1

73--77

EN

Twelve Sprague-Dawley rats were randomly divided into two groups: Citrus suavissima Hort. ex Tanaka group and control group (n 5 6). The rats in Citrus suavissima Hort. ex Tanaka group were given Citrus suavissima Hort. ex Tanaka juices (1 mL/100 g) by oral administration each day, continued for 14 days; the rats in control group were given Stroke-physiological saline solution (1 mL/100 g) by oral administration each day, continued for 14 days. The rats of these two groups were given a single oral administration of erlotinib (20 mg/kg) on the 15th day. After blood sampling at different time points and processing, the concentrations of erlotinib in rat plasma were determined by the established ultraperformance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method. Chromatographic separation was achieved using a UPLC BEH C18 column (2.1 mm 3 50 mm, 1.7 mm) with erlotinib-d6 as an internal standard (IS). The initial mobile phase consisted of acetonitrile and water (containing 0.1% formic acid) with gradient elution. Multiple reaction monitoring (MRM) modes were utilized to conduct quantitative analysis. The sensitive, rapid and selective UPLC-MS/MS method was successfully applied to analyse the effect of Citrus suavissima Hort. ex Tanaka on pharmacokinetics of erlotinib in rat plasma. There were no significant differences in AUC(0t), t1/2, Tmax, CL, Cmax between the two groups (P > 0.05). While MRT(0t) was decreased (P < 0.05) in Citrus suavissima Hort. ex Tanaka group, compared to the control group. It showed that Citrus suavissima Hort. ex Tanaka could not affect the metabolism of erlotinib.

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Determination of sarecycline by UPLC-MS/MS and its application to pharmacokinetic study in rats

Shen Yonghui, Meng Deru, Chen Feifei, Jiang Hui, Liming Hu, Zhou Yunfang, Zhang Miaomiao

Acta Chromatographica

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2021

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Vol. 33, no. 3

228--233

EN

Sarecycline is a narrow-spectrum antibiotic for the treatment of acne, which is a chronic inflammatory disease of the hair follicle sebaceous glands. In the study, UPLC-MS/MS was used to establish a rapid and accurate analytical method. The sarecycline was determined with poziotinib as internal standard (IS) in rat plasma. An ACQUITY UPLC HSS T3 column (2.1 × 100 mm, 1.8 μm) could performe chromatographic separation with the mobile phase (methanol: water of 0.1% formic acid) with gradient elution. The ions of target fragment were m/z 488.19→410.14 for sarecycline and m/z 492.06→354.55 for poziotinib, which could quantify the electrospray ionization of positive multiple reaction monitoring (MRM) mode. The linear calibration curve of the concentration range was 1–1,000 ng/mL for sarecycline with a lower limit of quantification (LLOQ) of 1 ng/mL. The mean recovery was between 82.46 and 95.85% for sarecycline and poziotinib in rat plasma. RSD for precision of inter-day and intra-day were between 3.24 and 13.36%, and the accuracy ranged from 105.26 to 109.75%. The developed and validated method was perfectly used in the pharmacokinetic study and bioavailability of sarecycline after intravenous and oral administration in rats.

17

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.