Wyniki wyszukiwania - Biblioteka Nauki

1

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

100%

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

|

tom 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.

2

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

100%

Weng Q. , Chen L. , Ye L. , Lu X. , Yu Z. , Wen C. , Chen R. , Huang G.

|

2019

|

tom 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.

3

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

88%

Wu H. , Lu M. , He J. , Huang M. , Zheng A. , Zhang M. , Wen C. , Ye J.

|

2019

|

tom 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%.

4

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

88%

Chen R. , Lu M. , Tu X. , Sun W. , Ye W. , Ma J. , Wen C. , Wang X. , Geng P.

|

tom 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.

5

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

88%

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

|

tom 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.

6

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

88%

Zhou Y. , Lu M. , Jiang J.

|

tom 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.

7

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

88%

Luo Y. , Li L. , Cai J. , Ma J. , Liu L. , Wang X. , Jin C.

|

2019

|

tom 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%.

8

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

75%

Chen S. , Ma J. , Wang X. , Geng P.

|

tom 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.