scholarly journals HPLC-MS/MS Analysis of Aconiti Lateralis Radix Praeparata and Its Combination with Red Ginseng Effect on Rat CYP450 Activities Using the Cocktail Approach

2020 ◽  
Vol 2020 ◽  
pp. 1-12
Author(s):  
Wenjuan Ma ◽  
Wei Wang ◽  
Xuhua Huang ◽  
Guangzhe Yao ◽  
Qi Jia ◽  
...  
Keyword(s):  
Heart Failure ◽  
Flow Rate ◽  
Chromatographic Separation ◽  
Mobile Phase ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Red Ginseng ◽  
Cocktail Approach

Red ginseng is often combined with Aconiti Lateralis Radix Praeparata to reduce alkaloids-related toxicity of the latter. Such herb-pairing also results in better therapeutic effect in heart failure, as compared to the singular use of either herb. The purpose of this study was to investigate the effect of Aconiti Lateralis Radix Praeparata and its combination with red ginseng on the activities of CYP450 enzymes in rats. A sensitive and reliable HPLC-MS/MS method was established and validated for the simultaneous determination of eight probe drugs, phenacetin (CYP1A2), tolbutamide (CYP2C9), omeprazole (CYP2C19), dextromethorphan (CYP2D6), dapsone (CYP3A4), 7-hydroxycoumarin (CYP2A6), bupropion (CYP2B6), and amodiaquine (CYP2C8), in rat plasma using diazepam as internal standard (IS). The chromatographic separation was performed on a Waters XBridge™ C18 column (2.1 mm × 100 mm, 3.5 μm) using a gradient elution with the mobile phase consisting of acetonitrile and water (containing 0.1% formic acid) at a flow rate of 0.3 mL/min. The method was successfully applied in evaluating the effect of Aconiti Lateralis Radix Praeparata and red ginseng on the activities of CYP450 enzymes. The pharmacokinetic results of the eight probe drugs suggested that Aconiti Lateralis Radix Praeparata may inhibit the activity of CYP2A6, CYP2C19, CYP2B6, CYP1A2, CYP3A4, and CYP2C9 enzymes in rats. Comparison between the two groups, Aconiti Lateralis Radix Praeparata combined with red ginseng and Aconiti Lateralis Radix Praeparata, indicated that red ginseng may inhibit the activity of CYP2D6 and CYP2B6 enzymes while inducing the activity of CYP1A2, CYP3A4, and CYP2C9 enzymes.

scholarly journals Development and validation of a rapid selective high-throughput LC-MS/MS method for the determination of triclabendazole sulfoxide concentrations in sheep plasma and its use in bioequivalence studies

2021 ◽  
Author(s):  
Lénárd Farczádi ◽  
Álmos Dósa ◽  
Orsolya Melles ◽  
Laurian Vlase
Keyword(s):  
Formic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Liver Fluke ◽  
Internal Standard ◽  
Gradient Elution ◽  
Sample Processing ◽  
Development And Validation ◽  
Analytical Separation

AbstractTriclabendazole is one of the main drugs used to treat liver fluke in livestock. A rapid LC-MS/MS method was developed and validated to determine ovine plasma levels of triclabendazole sulfoxide.A Gemini NX-C18 column was used to achieve analytical separation, with gradient elution of a mobile phase composed of 0.1% formic acid in acetonitril and 0.1% formic acid in water at flow rate of 0.6 mL/min. MRM with positive ESI ionization was used for the detection of triclabendazole sulfoxide (m/z 360.10 from m/z 376.97). Fenbendazole was used as internal standard. Plasma protein precipitation with acetonitrile was used for sample processing.The method was validated with regards to selectivity, linearity (r > 0.9939), within run and between run precision (CV < 8.9%) and accuracy (bias < 8.9%) over the concentration range 1–100 µg/mL plasma.The method developed is simple, selective and can be applied in bioequivalence and bioavailability studies.

Determination of Shanzhiside Methylester in Rat Plasma by Uplc-Ms/Ms and its Application to a Pharmacokinetic Study

2020 ◽  
Vol 16 (7) ◽  
pp. 960-966
Author(s):  
Qinghua Weng ◽  
Yichuan Chen ◽  
Zuoquan Zhong ◽  
Qianqian Wang ◽  
Lianguo Chen ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Precipitation Method ◽  
Reaction Monitoring ◽  
Limit Of Quantification ◽  
Pharmacokinetics In Rats

Introduction: In this study, we used UPLC-MS/MS to detect shanzhiside methylester in rat plasma, and investigated its pharmacokinetics in rats. Materials and Methods: Diazepam 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 methanol-0.1 % formic acid with gradient elution. Electrospray ionization (ESI) tandem mass spectrometry in multiple reaction monitoring (MRM) mode with positive ionization was applied. Results: The results indicated that within the range of 5-4000 ng/mL, linearity of shanzhiside methylester in rat plasma was acceptable (r>0.995), and the lower limit of quantification (LLOQ) was 5 ng/mL. Intra-day and inter-day precision RSD of shanzhiside methylester in rat plasma were lower than 14%. Accuracy range was between 87.3 % and 109.1 %, and matrix effect was between 99.2% and 106.3%. Conclusion: The method was successfully applied in the pharmacokinetics of shanzhiside methylester in rats after intravenous administration.

Determination of retinol, alpha-tocopherol, and beta-carotene in serum by liquid chromatography with absorbance and electrochemical detection.

1987 ◽  
Vol 33 (9) ◽  
pp. 1585-1592 ◽  
Author(s):  
W A MacCrehan ◽  
E Schönberger
Keyword(s):  
Electrochemical Detection ◽  
Chromatographic Separation ◽  
Protein Denaturation ◽  
Internal Standard ◽  
Beta Carotene ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Alpha Tocopherol ◽  
Phase Gradient

Abstract We describe a method for the determination of retinol, alpha-tocopherol, and beta-carotene in serum, using a liquid-chromatographic separation with wavelength-programmed ultraviolet/visible absorbance and amperometric electrochemical detection with a glassy carbon electrode. After protein denaturation and addition of an internal standard, tocol, 250-microL samples are twice extracted with hexane. The reversed-phase, gradient-elution chromatographic separation provides baseline resolution of: the all-trans isomer of retinol from the cis isomers, alpha- from gamma-tocopherol, and all-trans-beta-carotene from alpha-carotene and from cis-beta-carotene isomers. The linearity of response and the detection limits for the two detectors for the three analytes are measured. A comparison of the values obtained for serum extracts shows good agreement between the absorbance and electrochemical detectors.

A Novel LC-MS Method for the Determination of Abiraterone in Rat Plasma and its Application to Pharmacokinetic Studies

2021 ◽  
Vol 17 ◽  
Author(s):  
Linzhi Dai ◽  
Pei Lv ◽  
Yun He ◽  
Xiaoli Wang ◽  
Lili Chen ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Analytical Procedure ◽  
Internal Standard ◽  
Rat Plasma ◽  
Pharmacokinetic Studies ◽  
Quadrupole Mass ◽  
Limit Of Quantitation

Background: High–performance liquid chromatography (HPLC)–ultraviolet (UV) and liquid chromatography (LC)–mass spectrometry (MS)/MS methods have been used to analyse abiraterone (ART); however, a single-quadrupole mass spectrometer with LC-MS systems has never been used to analyse ART. Objective: The study aimed to establish a novel, simple assay of quantitating ART in rat plasma through LC–MS. Method: The analytical procedure involved the extraction of ART and D4-ART (internal standard, IS) from rat plasma through simple protein precipitation. Chromatographic separation was achieved using an isocratic mobile phase (acetonitrile: 5 mM ammonium formate with 0.1% formic acid, 50:50 v/v) at a flow rate of 0.30 mL/min on a Waters XBridge® C18 column with a total run time of 5 min. LC–MS ion transitions monitored were 350.1 and 354.1 for ART and IS, respectively. The method was validated, and the results met acceptance criteria. Results: The lower limit of quantitation achieved was 1 ng/mL, and linearity was 1–8000 ng/mL. The intra- and inter-day precisions were 1.26%–14.20% and 5.49%–13.08%, respectively, in rat plasma.

Determination of Paeoniflorin and Paeonol in Houyinan Tablet by UPLC

2012 ◽  
Vol 581-582 ◽  
pp. 68-72
Author(s):  
Chu Qin Yu ◽  
Hua Qing Lin ◽  
Yue Han Hou ◽  
Zhong Feng Shi ◽  
Di Shi Lin
Keyword(s):  
Quality Control ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Gradient Elution ◽  
The Other ◽  
Column Temperature ◽  
Average Recovery ◽  
Injection Volume

In this study, our purpose was to establish a UPLC method for the simultaneous determination of Paeoniflorin and Paeonol in Houyinan Tablet. The separation was performed on Acquity BEH C18 column(2.1mm×100mm,1.7μm), the mobile phase was acetonitrile-water with gradient elution at a flow rate of 0.2 mL•min-1, the detection wavelength was 230nm, the column temperature was 30°Cand the injection volume was 2μL. Paeoniflorin and Paeonol reached effective separation with the other components in this chromatographic conditions. Paeoniflorin and Paeonol were linear within the range of 0.0406~0.4064μg(r=0.9999) and 0.0426~0.4256μg (r=0.9999), respectively. The average recovery was 99.82% and 100.6%. The results of method validation indicated that the method was simple,quick,accurate, specific and less solvent consumption. It can be used for the quality control of Houyinan Tablet.

scholarly journals Application of RP-HPLC method for the simultaneous determination of cetirizine in the presence of quinolones

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Hina Shamshad ◽  
Agha Zeeshan Mirza
Keyword(s):  
Human Serum ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Diclofenac Sodium ◽  
Internal Standard ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines

Abstract Background Present work describes a fast, simple, and sensitive procedure for the simultaneous determination of cetirizine in the presence of quinolones using diclofenac sodium as an internal standard. The present work was designed to analyze these compounds in pharmaceutical and clinical labs being economical for use. Results The mobile phase consisted of the simple composition of methanol, acetonitrile, and water in a ratio of 50:20:30 with a pH adjusted to 3.1 at a flow rate of 1 mL min−1. The UV detection was performed at 225 nm. The linearity was assessed over the range of 2.5–50 μg mL−1 for all drugs. The parameters such as accuracy, precision, linearity (>0.999), and sensitivity were satisfactory. Conclusion The method was equally applicable for formulation and human serum with recovery values between 95 and 105%. The results of the method were validated statistically according to ICH guidelines.

scholarly journals Optimization of RP-HPLC method with UV detection for determination of ursodeoxycholic acid in pharmaceutical formulations

2020 ◽  
Vol 66 (1) ◽  
pp. 85-90
Author(s):  
Zhaklina Poposka Svirkova ◽  
Zorica Arsova-Sarafinovska ◽  
Aleksandra Grozdanova
Keyword(s):  
Ursodeoxycholic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Pharmaceutical Formulations ◽  
Gradient Elution ◽  
Hplc Method ◽  
Uv Detection ◽  
Rp Hplc ◽  
Ich Guidelines

Due to the low absorptivity of bile acids, the aim of this study was to develop and validate a simple and sensitive HPLC/UV method for quantification of ursodeoxycholic acid (UDCA) in pharmaceutical formulations. Effective separation was achieved on C18 end–capped column, with gradient elution of a mobile phase composed of 0.001 M phosphate buffer (pH 2.8±0.5) – acetonitrile mix, at flow rate 1.5 mL min-1, UV detection at 200 nm and injection volumes were 50 µL. The proposed HPLC method was fully validated according to the ICH guidelines and it was found to be simple, accurate, precise and robust. Key words: ursodeoxycholic acid, HPLC/UV, pharmaceutical formulations, validation

SIMULTANEOUS DETERMINATION OF PARACETAMOL, ACECLOFENAC AND TRAMADOL HYDROCHLORIDE IN PHARMACEUTICAL DOSAGE FORM BY RP-HPLC METHOD

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (01) ◽  
pp. 35-40
Author(s):  
Rajesh Sharma ◽  
◽  
Mukesh C. Sharma ◽  
Gaurav Vijaywargiya
Keyword(s):  
Flow Rate ◽  
Chromatographic Separation ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Tramadol Hydrochloride ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc

Chromatographic separation of paracetamol, aceclofenac and tramadol hydrochloride was performed on a Chromatopak C-18 column (25 cm x 4.6mm i.d. x 5µm) as stationary phase with a mobile phase composed of phosphate buffer pH 7.0: acetonitrile (65:35 V/V), pH 7.0 (adjusted with triethylamine) at flow rate of 1mL/min. Detection was carried out at 265 nm. The retention times of paracetamol, aceclofenac and Tramadol hydrochloride were found to be 2.7, 4.5 and 6.0 min, respectively. The proposed method was validated for linearity, accuracy, precision, LOD and LOQ. The method was found to be accurate, precise, specific, robust, and linear for the determination of paracetamol, aceclofenac and tramadol hydrochloride in pharmaceutical dosage form.

UPLC-ESI-MS/MS Method for Determination of Recombinant Antihypertensive Peptide in Rat Plasma

2015 ◽  
Vol 730 ◽  
pp. 254-259 ◽  
Author(s):  
Yan Li Cong ◽  
Shen Li ◽  
Bo Chen ◽  
Hai Yan Sun ◽  
Dong Liu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Mobile Phase ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Plasma Samples ◽  
Selected Ion Monitoring ◽  
Column Temperature ◽  
Qualitative And Quantitative ◽  
Esi Ms

The focus of the study was to establish an UPLC-ESI-MS/MS method for the qualitative and quantitative determination of VLPVPR in rat plasma. The method was as follows: Protein impurities in the rat plasma samples were precipitated with methanol; A Waters Acquity BEH C18 column (100 mm×2.1 mm, 1.7 μm) was adopted; the column temperature was 25°C; the mobile phase consisted of methanol-water with gradient elution at the steady flow rate of 0.3 mL·min-1; the detection wavelength was 202 nm. Mass spectrometry applied selected ion monitoring mode with m/z 255 (quantitative ion) and m/z 169 (qualitative ion). It was found that excellent linear relationship was obtained from the range of 10~200 ng·mL-1 (r=0.9991), the limit determination (LOD) of VLPVPR was 1.8 ng·mL-1, the recovery rate was 96.33%~100.76%, The inter and intre-day RSD were less than 7%. We thus conclude that a rapid and sensitive UPLC-ESI-MS/MS method was developed and validated for the determination of recombinant antihypertensive peptide VLPVPR in rat plasma. It can be applied to evaluate the pharmacokinetics of VLPVPR.

A Sensitive UPLC-MS/MS Method for the Determination of Flurbiprofen in Rat Plasma: Application to Real Sample

2021 ◽  
Author(s):  
Mehmet Emrah Yaman ◽  
Alptug Atila ◽  
Tugrul Cagri Akman ◽  
Mevlut Albayrak ◽  
Yucel Kadioglu ◽  
...  
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
High Sensitivity ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Negative Ion ◽  
Linear Calibration ◽  
Multiple Reaction Monitoring Mode

Abstract For the quantification of flurbiprofen in rat plasma, a simple UPLC-MS/MS method with high sensitivity and short retention time for flurbiprofen was developed and validated using specific parameters. Etodolac was used as internal standard. The transitions (precursor to the product) of flurbiprofen and internal standard were obtained using the electrospray ionization in the negative ion multiple reaction monitoring mode, 243.2 → 199.2, 286.2 → 212.1, respectively. For chromatographic separation, C18 column was used for the stationary phase and gradient elution was used for the mobile phase. This mobile phase consisted of a methanol (A) and a 5 mM ammonium formate solution (B), which varied at a flow rate of 0.4 mL/min. For flurbiprofen, LLOQ was determined as 5 ng/mL. Quantification of flurbiprofen in the rat plasma with a linear calibration curve of 5–5000 ng/mL (r &gt; 0.9991 for plasma) is possible with a retention time of 1.89 min. The total analysis time of the method was 3 min. The proposed method was validated. The intraday and inter-day precision (RSD%) and accuracy (RE%) were within 10% in all cases for flurbiprofen. The stability of flurbiprofen was evaluated under conditions such as short-term, long-term, autosampler and freeze/thaw. After method validation, flurbiprofen was succesfully quantified in real rat plasma samples.

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