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1

UPLC–MS/MS simultaneous determination of methamphetamine, amphetamine, morphine, monoacetylmorphine, ketamine, norketamine, MDMA, and MDA in hair

Chen Siyuan, Ma Jianshe, Wang Xianqin, Geng Peiwu

Acta Chromatographica

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2020

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Vol. 32, no. 2

145--148

EN

Hair is a stable specimen and has a longer detection window (from weeks to months) than blood and urine. Through the analysis of hair, the long-term information of the drug use of the identified person could be explored. Our work is to establish an ultra-performance liquid chromatography–tandem mass spectroscopy (UPLC–MS/MS) method for simultaneous determination of methamphetamine, amphetamine, morphine, monoacetylmorphine, ketamine, norketamine, 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyamphetamine (MDA) in hair. Methoxyphenamine was used as an internal standard. The chromatographic separation was performed on a UPLC ethylene bridged hybrid (BEH) C18 (2.1 mm × 50 mm, 1.7 μm) column using a mobile phase of acetonitrile–water with 10 mmol/L ammonium acetate solution which containing 0.05% ammonium hydroxide. The multiple reaction monitoring in positive electrospray ionization was used for quantitative determination. The intra-day and inter-day precisions (relative standard deviation [RSD]) were below 15%. The accuracy ranged between 85.5% and 110.4%, the average recovery rate was above 72.9%, and the matrix effect ranged between 92.7% and 109.2%. Standard curves were in the range of 0.05–5.0 ng/mg, and the correlation coefficients were greater than 0.995. The established UPLC–MS/MS method was applied to analyze the hair samples successfully.

2

Pharmacokinetics of ebeiedinone in mouse blood by UPLC–MS/MS

Jin Yongxi, Chen Yuyan, Liu Jiawen, Bao Xi, Zhi Yinghao, Wen Congcong, Zhu Wenzong

Acta Chromatographica

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2020

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Vol. 32, no. 3

194--198

EN

An ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was established to determine ebeiedinone in mouse blood, and the pharmacokinetics of ebeiedinone after intravenous (0.5 mg/kg) and oral (2, 4, and 8 mg/kg) administration was studied. Twenty-four mice were randomly divided into 4 groups, 1 group was for intravenous administration (0.5 mg/kg), and other 3 groups were for oral administration (2, 4, and 8 mg/kg), with 6 rats in each group. Yubeinine was used as an internal standard. Multiple reaction monitoring (MRM) mode was used to quantitatively analyzed ebeiedinone m/z 414.4 → 91.1 and the internal standard m/z 430.4 → 412.3 in the electrospray ionization (ESI) positive interface. In the concentration range of 1–2000 ng/mL, the ebeiedinone in the mouse blood was linear (r2 > 0.995), and the lower limit of quantification was 1.0 ng/mL. In the mouse blood, the intra-day precision coefficient of variation (CV) was less than 15%, and the inter-day precision CV was less than 15%. The accuracy ranged from 85.4% to 114.6%, and the average recovery was higher than 61.3%. The matrix effect was between 87.0% and 106.5%. These data met the pharmacokinetic study requirements of ebeiedinone. The UPLC–MS/MS method was sensitive, rapid, and selective and was successfully applied to the pharmacokinetic study of ebeiedinone in mice. The absolute bioavailability of ebeiedinone was 30.6%.

3

Development of an UPLC–MS/MS assay to determine psoralidin in rat plasma and its application in a pharmacokinetic study after intragastric administration

Feng Feng, Jiang Xiunan, Qiu Jieying, Wu Hongyu, Cai Xiaojun, Xiang Zheng

Acta Chromatographica

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2020

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Vol. 32, no. 4

215--218

EN

Psoralidin has a variety of pharmacological activities, such as anti-tumor, anti-depressant, and anti-inflammatory activities. This study aims at developing a rapid ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method to determine psoralidin in rat plasma and studying the pharmacokinetic characteristic of psoralidin after intragastric administration of 20 and 40 mg/kg. Alpinetin was used as an internal standard (IS), and the plasma samples were precipitated with acetonitrile. The calibration curves were linear over the range of 0.2–250 ng/mL (R2 = 0.993). The pharmacokinetic parameters were calculated by DAS 3.0. Half-life (t1/2) was 7.2 ± 0.97 h and 7.1 ± 0.27 h for different dosages, respectively. Tmax was 4.2 ± 1.1 h and 4.0 ± 1.1 h for different dosages, respectively. Apparent volume of distribution (Vd) for different dosages was 630.1 ± 168.8 and 600.1 ± 138.8 L/kg, respectively. Clearance (CL) was 105.6 ± 29.2 and 100.6 ± 22.2 L/h/kg for different dosages, indicating that psoralidin was mainly distributed in rat tissues. The pharmacokinetic study provided important information for further clinical application in the treatment of cancer and osteoporosis.

4

Simultaneous determination of atractylenolide I and II in rat plasma by UPLC–MS/MS and its application to pharmacokinetic study after intravenous administration

Chen Lianguo, Wu Haiya, Tu Xiaoting, Zhao Yi, Jiang Yanyan, Wen Congcong, Luo Yue

Acta Chromatographica

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2019

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Vol. 31, no. 1

8--11

EN

Atractylodis exerted a variety of pharmacological effects such as anti-tumor, anti-inflammatory, anti-bacterial, and anti-aging effects etc. The major ingredients of Atractylodis are atractylenolide I and II that exhibited activities in anti-inflammatory and anticancer. In this work, a sensitive and selective ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method for determination of atractylenolide I and II in rat plasma was developed. The UPLC–MS/MS method was validated for selectivity, linearity, accuracy, precision, recovery, and stability with a total run time of 4.0 min. After addition of atractylenolide III as an internal standard (IS), protein precipitation by acetonitrile was used to prepare samples. Chromatographic separation was achieved on a UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) with 0.1% formic acid and acetonitrile as the mobile phase with gradient elution. An electrospray ionization source was applied and operated in positive ion mode; multiple reactions monitoring (MRM) mode was used for quantification using target fragment ions m/z 231.1 → 185.1 for atractylenolide I, m/z 233.1 → 91.0 for II, and m/z 249.0 → 231.1 for IS. Calibration plots were linear throughout the range 1–1000 ng/mL for atractylenolide I and II in rat plasma. Mean recoveries of atractylenolide I and II in rat plasma ranged from 86.2% to 96.3%. Relative standard deviation (RSD) of intra-day and inter-day precision was both less than 12%. The accuracy of the method was between 91.0% and 109.0%. The method was successfully applied to pharmacokinetic study of atractylenolide I and II after intravenous administration in rats.

5

Pharmacokinetics of panasenoside in rats and tissue distribution in mice by ultra-performance liquid chromatography tandem mass spectrometry

Chen Ruijie, Lu Mengrou, Tu Xiaoting, Sun Wei, Ye Weijian, Ma Jianshe, Wen Congcong, Wang Xianqin, Geng Peiwu

Acta Chromatographica

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2019

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Vol. 31, no. 2

146--150

EN

We developed an ultra-performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS) method for quantification of panasenoside pharmacokinetics in rat plasma and tissue distribution in mouse. Twelve male Sprague-Dawley rats were used for pharmacokinetics after intravenous (2 or 10 mg/kg) administration of panasenoside, six rats for each dose. Thirty mice were randomly divided into six groups (five mice for each group, one group for each time point) and received 20 mg/kg of panasenoside by intraperitoneal administration. Calibration plots were in the range of 2–2000 ng/mL for panasenoside in rat plasma and 2–3000 ng/mL in mouse tissues. The relative standard deviation (RSD) of inter-day and intra-day precision was less than 14%. The accuracy was between 89.6% and 110.0%. The AUC(0-t) was 160.8 ± 13.0 and 404.9 ± 78.0 ng/mL*h, and t1/2 of 3.2 ± 1.2 and 4.6 ± 1.7 h, CL (clearance) of 10.0 ± 2.0, and 21.4 ± 2.0 L/h/kg after intravenous administration 2 mg/kg and 10 mg/kg of panasenoside, respectively. The tissue distribution results indicated that the panasenoside diffuses rapidly and widely into major organs. The level of panasenoside was highest in mouse liver, followed by kidney, lung, and spleen. The overwhelming accumulation in liver indicated that liver was responsible for the extensive metabolism.

6

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.

7

Pharmacokinetic study on hirsutine and hirsuteine in rats using UPLC–MS/MS

Han Aixia, Lin Guanyang, Cai Jinzhang, Wu Qing, Geng Peiwu, Ma Jianshe, Wang Xianqin, Lin Chongliang

Acta Chromatographica

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2019

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Vol. 31, no. 2

99--104

EN

An ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was established to determine hirsutine and hirsuteine in rat plasma. Pharmacokinetics of hirsutine and hirsuteine in rats after intravenous or oral administration has been investigated using this developed UPLC–MS/MS method, and bioavailability of the two drugs was calculated. Diazepam was used as internal standard, and UPLC BEH column (2.1 mm × 50 mm, 1.7 μm) was used at temperature of 40 °C. The mobile phase was composed of acetonitrile and water (containing 0.1% formic acid) at a gradient elution flow rate of 0.4 mL/min. Nitrogen was used as desolvation gas (800 L/h) and conical gas (50 L/h). The multiple reaction monitoring (MRM) model was applied to quantitatively analyze hirsutine m/z 369 → 226, hirsuteine m/z 367 → 169.9, and diazepam (internal standard) m/z 285.1 → 193.3. Rat plasma samples were deproteinized using acetonitrile prior to UPLC–MS/MS analysis. Within the concentration range of 1–200 ng/mL, the linearity of hirsutine and hirsuteine in plasma was good (r > 0.995), and the lower limit of quantitation was 1 ng/mL. Relative standard deviations of intra-day precision for hirsutine and hirsuteine were ≤6.1% and ≤5.9%, respectively, and those of inter-day precision were ≤6% and ≤7.7%. Accuracy for hirsutine and hirsuteine ranged between 92.3% and 104.8%. Bioavailability of hirsutine and hirsuteine was 4.4% and 8.2%, respectively. The method is sensitive and fast with good selectivity and was successfully applied in the pharmacokinetic studies after intravenous and oral administration of hirsutine and hirsuteine.

8

Determination of RKI-1447 in rat plasma by UPLC–MS/MS and investigation on its pharmacokinetics, an effective ROCK1 and ROCK2 inhibitor

Luo Yue, Li Liyi, Cai Jinzhang, Ma Jianshe, Liu Le, Wang Xianqin, Jin Chun

Acta Chromatographica

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2019

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Vol. 31, no. 3

211--215

EN

RKI-1447 is an effective ROCK1 and ROCK2 inhibitor, having anti-invasion and anti-tumor activity. In this study, we used ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) to detect RKI-1447 in rat plasma and investigated its pharmacokinetics in rats. Diazepam was utilized as an internal standard, and an acetonitrile precipitation method was used to process the plasma samples. Chromatographic separation was achieved using a UPLC ethylene bridged hybrid (BEH) column (2.1 mm × 50 mm, 1.7 μm) with a gradient acetonitrile–water mobile phase (containing 0.1% formic acid). Flow rate was set at 0.4 mL/min. Electrospray ionization (ESI)–tandem mass spectrometry in multiple reaction monitoring (MRM) mode with positive ionization was applied: m/z 327.1 → 204.0 and 285.1 → 193.3 for RKI-1447 and internal standard, respectively. The results indicated that within the range of 10–2000 ng/mL, the linearity of RKI-1447 in rat plasma was acceptable (r > 0.995), and the lowest limit of quantification (LLOQ) was 10 ng/mL. Intra-day precision RSD of RKI-1447 in rat plasma was lower than 8%, and inter-day precision RSD was lower than 11%. Accuracy range was between 91.6% and 107.1%, and the matrix effect was between 85.1% and 87.0%. The analysis method was sensitive and fast with suitable selectivity, and was successfully applied in the pharmacokinetics of RKI-1447 in rats. The bioavailability of the RKI-1447 was 7.3%.

9

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.

10

Determination of benzoxazinoids in Spring and Winter varieties of wheat using ultra-performance liquid chromatography coupled with mass spectrometry

Kowalska I., Kowalczyk M.

Acta Chromatographica

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2019

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Vol. 31, no. 3

179--182

EN

The composition and concentration of natural products largely depend on a plant part, development stage, cultivar, and growing conditions. This study evaluated the influence of cultivars and production systems on the composition of natural products (benzoxazinoids) in wheat aerial parts. The determination of benzoxazinoids was performed by combining pressurized liquid extraction, ultra-performance liquid chromatography, and tandem mass spectrometry. Six benzoxazinoids were identified and quantitated in wheat varieties. Significant differences were observed among the examined varieties. The average concentrations of total researched compounds were definitely higher in the organically produced spring wheat cultivars than in the winter ones. The content of these compounds in the same varieties grown under organic and conventional systems showed their higher content under the organic one. The main benzoxazinoids detected in wheat varieties were 2,4-dihydroxy-7-methoxy-1,4-benzoxazin-3-one glucoside (DIMBOA-Glc) and 6-methoxy-2-benzoxazolinone (MBOA). The richest sources of benzoxazinoids were Brawura, Łagwa, and Kandela (52.46, 34.67, and 30.14 μg/g dry weight [DW], respectively).

11

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

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2019

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Vol. 31, no. 3

222--227

EN

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%.

12

Effect of curcumin and pirfenidone on toxicokinetics of paraquat in rat by UPLC–MS/MS

Wang S., Lin Z., Su K., Zhang J., Zhang L., Gao Z., Ma J., Wang X.

Acta Chromatographica

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2018

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Vol. 30, no. 1

26--30

EN

The rats were randomly divided into paraquat group, curcumin treatment group, and pirfenidone treatment group. The concentration of paraquat in rat plasma was determined by an ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method over the range of 10–2000 ng mL−1. Chromatographic separation was achieved on a BEH HILIC (2.1 mm × 100 mm, 1.7 μm) column. The mobile phase was consisted of acetonitrile and 10 mm ammonium formate buffer (containing 0.1% formic acid) with gradient elution pumped at a flow rate of 0.4 mL min−1. Protein precipitation with acetonitrile was used as sample preparation. Compared with the paraquat group, there is statistical toxicokinetic difference for curcumin treatment group and pirfenidone treatment group, AUC(0 − t) decreased (P < 0.05), clearance (CL) increased (P < 0.05) for curcumin or pirfenidone treatment group, and Cmax decreased (P < 0.05) for curcumin treatment group. The results showed that treatment by curcumin and pirfenidone could relieve acute paraquat poisoning in rats.

13

Development of UPLC–MS/MS method for quantitative analysis of curcumin in human plasma

Hayun H., Rahmawati R., Harahap Y., Sari S.

Acta Chromatographica

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2018

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Vol. 30, no. 4

207--211

EN

A specific, very rapid, and sensitive ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method for quantitative analysis of curcumin in human plasma has been developed and validated. Diazepam was used as internal standard (IS). The analytes were isolated using liquid–liquid extraction method with the mixture of ethyl acetate–methanol (95:5). The organic solvents were evaporated, reconstituted in mobile phase, and injected to UPLC completed with UPLC BEH C18 column 1.7 μm, 2.1 × 100 mm Acquity® Waters as stationary phase, mixture of 0.15% formic acid–acetonitril (50:50, v/v) as mobile phase, and flow rate of 0.5 mL/min and detected in positive ionization mode tandem mass spectrometer operated in multiple reaction monitoring (MRM). The MS/MS ion transitions monitored were m/z 369.05 → 176.95 and 284.95 → 193 for curcumin and IS, respectively. The retention times for curcumin and IS were 1.7 and 1.4 min, respectively, and the linearity range was 1–100 ng/mL with a coefficient correlation (r) of 0.999 and lower limit of quantitation (LLOQ) of 1 ng/mL. The relative standard deviation (RSD) values of the intra- and inter-assay precisions of the method were below 8.3% and 12.7%, respectively, while the accuracy ranged from 89.5 to 98.7% and the extraction recovery of curcumin and IS was up to 86.6%. The data presented show that the method provides specific, very rapid, sensitive, precise, and accurate measurements of curcumin concentrations in human plasma.

14

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.

15

Determination of silodosin in biological samples using UPLC–MS/MS combined with magnetic carboxylated multiwalled carbon nanotubes

Yin Q. H., Zhu Y. Q., Yang Y. L.

Acta Chromatographica

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2018

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Vol. 30, no. 1

47--53

EN

Novel magnetic solid-phase extraction using carboxylated multiwalled carbon nanotubes was proposed with ultra high-performance liquid chromatography–tandem mass spectrometry for the determination of silodosin in biological samples. The effects of various experimental parameters including adsorbent amount, pH, adsorption time, desorption conditions, and adsorbent reusability were systematically validated. Under the optimized conditions, the calibration curve was linear within the concentration range of 1.0–800 ng mL−1 with the correlation coefficient of 0.9997 and the lower limit of detection was 0.3 ng mL−1. The extraction recoveries were over 90.0% with relative standard deviation (RSD) of less than 5.0%. All these results suggested that magnetic extraction method can be used for enrichment and quantification of silodosin in biological samples.

16

Determination and pharmacokinetic study of jaceosidin in rat plasma by UPLC–MS/MS

Zhou Y., Chen B., Chen J., Dong Y., Wang S., Wen C., Wang X.

Acta Chromatographica

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2018

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Vol. 30, no. 2

131--135

EN

In this work, a sensitive and selective ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed and fully validated for determination of jaceosidin in rat plasma. Avicularin was used as the internal standard (IS), and protein precipitation by acetonitrile was used to prepare samples. Chromatographic separation was achieved on a UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 μm) with 0.1% formic acid and acetonitrile as the mobile phase with gradient elution. An electrospray ionization (ESI) source was applied and operated in positive ion mode; multiple reaction monitoring (MRM) mode was used for quantification. Calibration plots were linear throughout the range 2–500 ng Ml-1 for jaceosidin in rat plasma. Relative standard deviation (RSD) of intra-day and inter-day precision was less than 12%. The accuracy of the method was between 88.7% and 109.7%. Mean recoveries of jaceosidin in rat plasma ranged from 65.4% to 77.9%. The developed UPLC–MS/MS method was successfully applied to pharmacokinetic study of jaceosidin after intravenous administration of 2 mg kg-1 in rats. We could find that the jaceosidin rapidly eliminated, the t1/2 was 0.7 ± 0.3 h, and clearance (CL) was 22.4 ± 3.0 L h-1 kg-1.

17

Determination and pharmacokinetic study of dauricine in rat plasma by UPLC–MS/MS

Geng P., Zhang J., Chen B., Wang Q., Wang S., Wen C.

Acta Chromatographica

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2018

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Vol. 30, no. 2

136--140

EN

Dauricine is the major bioactive component isolated from the roots of Menispermum dauricum D.C., a bisbenzylisoquinoline alkaloid derivative, and has shown multiple pharmacological properties. In this work, a sensitive and selective ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed for determination of dauricine in rat plasma and its application to pharmacokinetic study of dauricine after intravenous and oral administration in rats. After addition of daurisoline as an internal standard (IS), protein precipitation by acetonitrile was used to prepare samples. Chromatographic separation was achieved on a UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) with 0.1% formic acid and acetonitrile as the mobile phase with gradient elution. An electrospray ionization source was applied and operated in positive ion mode; multiple reactions monitoring (MRM) mode was used for quantification. Calibration plots were linear throughout the range 2–600 ng mL−1 for dauricine in rat plasma. Relative standard deviation (RSD) of intra-day and inter-day precision was less than 13%. The accuracy of the method was between 95.8% and 105.9%. Matrix effect of dauricine in rat plasma ranged from 88.0% to 90.3%. Mean recoveries of dauricine in rat plasma ranged from 91.5% to 95.1%. The method was successfully applied to pharmacokinetic study of dauricine after intravenous and oral administration in rats. The bioavailability of dauricine was found to be 55.4% for the first time.

18

A rapid and sensitive UPLC–MS/MS method for determination of remimazolam and its main metabolite in human urine and its application in clinical urine recovery study

Zhou Y., Lu M., Jiang J.

Acta Chromatographica

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2018

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Vol. 30, no. 2

109--113

EN

Remimazolam is a new chemical entity belonging to the benzodiazepine class of sedative drugs. A sensitive and rapid method based on ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) has been developed and validated for the determination of remimazolam and its major carboxylic acid metabolite (M1) in human urine. Urine samples were prepared by dilution and analyzed using an isocratic chromatographic separation. Inter- and intra-batch results for remimazolam were within 10.7% for accuracy and 5.5% for precision, and for M1, within 5.8% for accuracy and 4.2% for precision, respectively. This study represents the first reported example for the quantification of remimazolam and its main metabolite in human urine. Furthermore, this method has been successfully applied for the urine recovery study of remimazolam in Chinese healthy subjects. Only about 0.01% of the administered remimazolam dose was eliminated in the urine over the 24 h period in the form of unchanged remimazolam, and more than 75.1% of the administered dose was eliminated in the form of M1. Remimazolam is excreted mainly in the form of M1 in urine after intravenous administration, and there is no excessive accumulation in vivo after administration of remimazolam.