Development and Validation of an LC-MS/MS Method for Simultaneous Determination of Canagliflozin and Metformin HCl in Rat Plasma and its Application

2020 ◽  
Vol 16 (6) ◽  
pp. 752-762
Author(s):  
Vivek Nalawade ◽  
Vaibhav A. Dixit ◽  
Amisha Vora ◽  
Himashu Zade
Keyword(s):  
Internal Standard ◽  
Rat Plasma ◽  
Precipitation Method ◽  
Herbal Extracts ◽  
One Step ◽  
Precision And Accuracy ◽  
Development And Validation ◽  
The Impact ◽  
Metformin Hcl

Background: Food and herbal extracts rich in Quercetin (QRT) are often self-medicated by diabetics and can potentially alter the pharmacokinetics (PK) of Metformin HCl (MET) and Canagliflozin (CNG) leading to food or herb-drug interactions and reduced therapeutic efficacy. However, the impact of these flavonoids on the pharmacokinetic behaviour of MET and CNG is mostly unknown. Methods: A simple one-step protein precipitation method was developed for the determination of MET and CNG from rat plasma. The mobile phase chosen was MeOH 65% and 35% water containing 0.1% formic acid at a flow rate of 1mL/min. Results: The retention time of MET, internal standard (Valsartan) and CNG was 1.83, 6.2 and 8.2 min, respectively. The method was found to be linear in the range of 200 - 8000 ng/mL for CNG and 100 = 4000 ng/ml for MET. Precision and accuracy of the method were below 20% at LLOQ and below 15% for LQC, MQC, and HQC. Conclusion: The method was successfully applied for the determination of PK of MET and CNG by using 100 μL of rat plasma. QRT co-administration affects the PK parameters of MET and CNG. This alteration in PK parameters might be of significant use for clinicians and patients.

scholarly journals Determination of diosmetin-7-o-β-d-glucoside in rat plasma by UPLC–MS/MS

2020 ◽  
Vol 32 (4) ◽  
pp. 264-268
Author(s):  
Jianbo Li ◽  
Zheng Yu ◽  
Cheng Han ◽  
Zhening Wang ◽  
Yujie Hu ◽  
...  
Keyword(s):  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Precipitation Method ◽  
Reaction Monitoring ◽  
Caudal Vein ◽  
One Step ◽  
Pharmacokinetics In Rats

In this study, we used UPLC–MS/MS to determine diosmetin-7-o-β-d-glucoside in rat plasma and investigated its pharmacokinetics in rats. Six rats were given diosmetin-7-o-β-d-glucoside (5 mg/kg) by intravenous (i.v.) administration. The blood (150 μL) was withdrawn from the caudal vein after administration. Diazepam was used as an internal standard (IS), and a one-step acetonitrile precipitation method was used to process the plasma samples. Chromatographic separation was achieved using a UPLC BEH C18 column using a 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, 463.1 → 301.0 for diosmetin-7-o-β-d-glucoside, m/z 285.1 → 193.0 for diazepam (IS). Intra-day and inter-day precision of diosmetin-7-o-β-d-glucoside in rat plasma were less than 14%. The method was successfully applied in the pharmacokinetics of diosmetin-7-o-β-d-glucoside in rats after intravenous administration. The t1/2 of diosmetin-7-o-β-d-glucoside is 1.4 ± 0.4 h, which indicates the quick elimination.

scholarly journals Development and validation of a simple bio-analytical HPLC-UV method for estimation of irbesartan in human plasma

2020 ◽  
Vol 11 (3) ◽  
pp. 3846-3849
Author(s):  
Ashok P ◽  
Narenderan S T ◽  
Meyyanathan S N ◽  
Babu B ◽  
Jawahar N
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
High Performance ◽  
Internal Standard ◽  
Precipitation Method ◽  
Quantification Limit ◽  
Us Fda ◽  
Development And Validation ◽  
Analytical Hplc

The present study was aimed to develop and validate a simple, sensitive and economical bio-analytical high-performance liquid chromatographicultraviolet method for the determination of irbesartan in human plasma. The method involves the use of simple precipitation method for the determination of irbesartan, using methanol as precipitating agent and losartan as internal standard. The separation was achieved using Zorbax C18 column (150 x 4.6 mm, 5µm), mobile phase consists of methanol and 0.2% formic acid in water at the ratio 85:15, v/v using detection wavelength of 237 nm. Further, the developed method was validated as per US-FDA guidelines for accuracy, precision, linearity, stability, detection and quantification limit. The method developed was found to be linear over the concentration ranging from 5 to 500 ng/ml with a correlation coefficient of 0.9987. The LOD and LLOQ of the method were found to be 1 ng/ml and 5 ng/ml, respectively.

scholarly journals Development and Validation of an HPLC/MS/MS Method for Determining the Thiazolidinone PG15 in Rat Plasma

2010 ◽  
Vol 93 (4) ◽  
pp. 1215-1221
Author(s):  
FláVia D T UchôA ◽  
Eduardo C Palma ◽  
Natalia F Souza ◽  
Maria C A Lima ◽  
Suely L Galdino ◽  
...  
Keyword(s):  
Internal Standard ◽  
Ammonium Hydroxide ◽  
Rat Plasma ◽  
Negative Ion ◽  
Pharmacokinetic Studies ◽  
Plasma Samples ◽  
Isocratic Elution ◽  
Negative Ion Mode ◽  
Development And Validation

Abstract A rapid, sensitive, and simple HPLC/MS/MS method was developed and validated for the determination of (5Z,E)-3-[2-(4-chlorophenyl)-2-oxoethyl]-5-(1H-indol-3-ylmethylene)-thiazolidine-2, 4-dione (PG15) in rat plasma using chlortalidone as an internal standard (IS). Analyses were performed using a C18 column and isocratic elution with acetonitrilewater (90 + 10, v/v) containing 10 mM ammonium hydroxide (pH 8.0) as the mobile phase pumped at 0.3 mL/min. Detection was performed by MS with negative ion mode electrospray ionization. Rat plasma samples were prepared by deproteinizing with acetonitrile. Detected fragments were 395.1 > 171.9 for PG15 and 337.3 > 189.9 for the IS. Calibration curves were linear from 10 to 1000 ng/mL, with the determination coefficient >0.99. The intraday and interday precisions were less than 12.2 and 11.3, respectively. The applicability of the HPLC/MS/MS method for pharmacokinetic studies was tested using plasma samples obtained after oral administration of PG15 to rats, and it provided the necessary sensitivity, linearity, precision, accuracy, and specificity.

scholarly journals HPLC Method Determination of Isoliquiritin Apioside and Isoliquiritin in Rat Plasma for Application in Pharmacokinetic Study after an Oral Administration of Zhigancao Extract

2012 ◽  
Vol 2012 ◽  
pp. 1-6 ◽  
Author(s):  
Yan-yun Yang ◽  
Liang Xu ◽  
Song-yao Hao ◽  
Yan Li ◽  
Zhen-Qiu Zhang
Keyword(s):  
Oral Administration ◽  
Pharmacokinetic Study ◽  
Mobile Phase ◽  
Internal Standard ◽  
Rat Plasma ◽  
Hplc Method ◽  
Plasma Samples ◽  
Limit Of Quantification ◽  
Precision And Accuracy

A sensitive HPLC method was developed for the quantitative determination of isoliquiritin apioside (ILA) and isoliquiritin (IL) in rat plasma. After protein precipitation with acetonitrile, chloroform was used to separate lipid-soluble impurities from the plasma samples and remove acetonitrile. A chromatography was carried out on Diamonsil C18 (150×4.6 mm; 5 μm) analytical column, using a mobile phase consisting of water (containing phosphoric acid 0.1%, v/v); acetonitrile (72 : 28, v/v) at a flow rate of 1.0 mL/min. The wavelength-switching technology was performed to determine ILA and IL at 360 nm and wogonoside (internal standard, IS) at 276 nm. The calibration curves of ILA and IL were fairly linear over the concentration ranges of 0.060–3.84 μg/mL (r=0.9954) and 0.075–4.80 μg/mL (r=0.9968), respectively. The average extract recoveries of ILA, IL, and IS were all over 80%. The precision and accuracy for all concentrations of quality controls and standards were within 15%. The lower limit of quantification (LLOQ) was 0.060 μg/mL for ILA and 0.075 μg/mL for IL. The method was used in pharmacokinetic study after an oral administration of Zhigancao extract to rats.

scholarly journals Desarrollo y validación de un método analítico para la determinación de ciprofloxacina en suero por cromatografía liquida de alta precisión con detección ultravioleta./ development and validation of an analytical method for the determination of ciproflox

2013 ◽  
Vol 13 (2) ◽  
pp. 119-126
Author(s):  
Ana Falquez Manotas ◽  
Luz adriana Sarmiento Rubiano
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Pharmacokinetic Studies ◽  
Simple Method ◽  
Ultraviolet Detection ◽  
Precision And Accuracy ◽  
The Times ◽  
Development And Validation ◽  
Antibacterial Spectrum

Objetivo: Desarrollar un método rápido y sencillo para la determinación de Ciprofloxacina en muestras de suero para ser utilizado en estudios farmacocinéticos. La Ciprofloxacina es un antibiótico que pertenece al grupo de las fluoroquinolonas, comúnmente usado en Colombia con un amplio espectro antibacterial. Diferentes métodos utilizando Cromatografía Liquida de Alta precisión (HPLC) han sido reportados para el análisis de Ciprofloxacina en fluidos biológicos. Materiales y métodos: Se empleó el método Cromatografía Liquida de Alta Precisión (HPLC) con detección ultravioleta a 280 nm, fase móvil isocrática, Dexametasona como estándar interno y un rango de cuantificación de 0,1 a 10 μg/ml. Resultados: Los tiempos de retención fueron 4,93 min y 15,71 minutos para Ciprofloxacina y Dexametasona respectivamente, la precisión y exactitud fueron superiores al 95% y el tiempo total de elución fué de 20 minutos por muestra. Conclusiones: Se desarrolló y validó un método analítico para la determinación de Ciprofloxacina en suero, lo suficientemente sensible, exacto, y reproductible para ser usado en estudios farmacocinéticos. Objective: To develop a rapid and simple method for Ciprofloxacin determination insamples of whey to be used in pharmacokinetic studies. Ciprofloxacin is an antibioticthat belongs to the group of the fluoroquinolone, commonly used in Colombia with anextensive antibacterial spectrum. Several High-Performance Liquid Chromatography(HPLC) methods have been reported for the analysis of ciprofloxacin in biologicalfluids. Materials and methods: the method used was High-Performance LiquidChromatography (HPLC) with ultraviolet detection to 280 nm, mobile phase isocratic,Dexamethasone as internal standard and a range of quantification from 0,1 to 10 μg/ml. Results: The times of retention were 4,93 min and 15,71 min for Ciprofloxacin andDexamethasone respectively, precision and accuracy were More than 95 % and a andelution time per sample was 20 minutes. Conclusions: Was developed and validateda sensitive and accurate analytical methods for Ciprofloxacin determination in serum,It is the sufficiently reproducible to be used in pharmacokinetic studies

scholarly journals Determination and pharmacokinetics of calycanthine in rat plasma by UPLC-MS/MS

2020 ◽  
Author(s):  
Meifei Lu ◽  
Xiaojie Lu ◽  
Zheng Yu ◽  
Congcong Wen
Keyword(s):  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Precipitation Method ◽  
Absolute Bioavailability ◽  
Limit Of Quantification ◽  
The Matrix ◽  
Acid Aqueous Solution

AbstractCalycanthine 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 × 2.1 mm, 1.7 μm) 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.

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.

scholarly journals Bioanalytical Method Development and Validation of Veratraldehyde and Its Metabolite Veratric Acid in Rat Plasma: An Application for a Pharmacokinetic Study

Molecules ◽  
2020 ◽  
Vol 25 (12) ◽  
pp. 2800
Author(s):  
Hyun Wook Huh ◽  
Hee-Yong Song ◽  
Young-Guk Na ◽  
Minki Kim ◽  
Mingu Han ◽  
...  
Keyword(s):  
Method Development ◽  
Internal Standard ◽  
Rat Plasma ◽  
Precipitation Method ◽  
Veratric Acid ◽  
Bioanalytical Method ◽  
Positive Mode ◽  
Percutaneous Administration ◽  
The One

A simple, sensitive, and rapid UHPLC-MS/MS method was developed for the simultaneous determination of veratraldehyde and its metabolite veratric acid in rat plasma. Cinnamaldehyde was used as an internal standard (IS) and the one-step protein precipitation method with 0.2% formic acid in acetonitrile (mobile phase B) was used for the sample extraction. Reversed C18 column (YMC-Triart C18 column, 50 mm × 2.0 mm, 1.9 µm) was used for chromatographic separation and was maintained at 30 °C. The total run time was 4.5 min and the electrospray ionization in positive mode was used with the transition m/z 167.07 → 139.00 for veratraldehyde, m/z 183.07 → 139.00 for veratric acid, and m/z 133.00 → 55.00 for IS. The developed method exhibited good linearity (r2  ≥  0.9977), and the lower limits of quantification ranged from 3 to 10 ng/mL for the two analytes. Intra-day precision and accuracy parameters met the criteria (within ±15%) during the validation. The bioanalytical method was applied for the determination of veratraldehyde and veratric acid in rat plasma after oral and percutaneous administration of 300 and 600 mg/kg veratraldehyde. Using the analytical methods established in this study, we can confirm the absorption and metabolism of veratraldehyde in rats for various routes.

scholarly journals Simultaneous Determination of Ten Bioactive Components from Shenling Baizhu San in Rat Plasma by UHPLC-MS/MS: Application to a Comparative Pharmacokinetic Study in Normal and Two Models of Ulcerative Colitis Rats

2021 ◽  
Vol 2021 ◽  
pp. 1-15
Author(s):  
Xia Xu ◽  
Weiwei Wang ◽  
Yaxi Chen ◽  
Qiyun Zhang ◽  
Bingtao Li ◽  
...  
Keyword(s):  
Ulcerative Colitis ◽  
Simultaneous Determination ◽  
Internal Standard ◽  
Rat Plasma ◽  
Scientific Basis ◽  
Precipitation Method ◽  
Pharmacokinetic Parameters ◽  
Spleen Deficiency ◽  
Validation Parameters

Shenling Baizhu San, a traditional formula, has a long history of treating spleen asthenic diarrhea by invigorating the spleen and dispelling dampness in China. A rapid and accurate UHPLC-MS/MS method was developed and fully validated for the simultaneous determination of ten active constituents in rat plasma: panaxadiol, ginsenoside Rg1, atractylenolide I, atractylenolide III, pachymic acid, neferine, nuciferine, diosgenin, platycodin D, and isoliquiritigenin. The plasma samples were pretreated by the protein precipitation method with acetonitrile. The analytes and puerarin (internal standard) were determined with high selectivity and sensitivity (LLOQ, 0.31–0.68 ng·mL−1) within 10 minutes. The validation parameters, including intra-/interday precisions, accuracy, recovery, matrix effect, and stability, were within acceptable ranges. The validated method was successfully applied to the pharmacokinetics study of ten components in normal and two rat models of ulcerative colitis (i.e., spleen deficiency with dampness retention-ulcerative colitis (SDDR-UC) rats and pure-ulcerative colitis (P-UC) rats). The pharmacokinetic parameters were significantly different among the three groups of rats. Overall, the absorption of the components was shown as follows: normal group > SDDR-UC group > P-UC group. The study could provide a scientific basis for further studies on pharmacokinetics and clinical differential application of SDDR-UC and P-UC patients.

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