scholarly journals Bio-Analytical Method Development of Repaglinide Drug Delivery Systems

2019 ◽  
Vol 9 (6) ◽  
pp. 140-142
Author(s):  
B. Ramu ◽  
Kaushal K Chandrul ◽  
P. Shanmuga Pandiyan
Keyword(s):  
Phosphate Buffer ◽  
Extraction Method ◽  
Mobile Phase ◽  
High Performance ◽  
Drug Delivery Systems ◽  
Method Development ◽  
Extraction Efficiency ◽  
Ultraviolet Spectroscopy ◽  
Rabbit Plasma ◽  
Solvent Extraction Method

A sensitive, specific and rapid high-performance liquid chromatography-ultraviolet spectroscopy method was developed and successfully validated to estimate the repaglinide in rabbit plasma. The solvent extraction method was used for  repaglinide from serum by using ethyl acetate and 0.1N HCl. The mobile phase consists of acetonitrile: phosphate buffer pH 4.0 at 60:40 %v/v with 1% triethylamine at flow rate of 0.8ml/min and at fixed wavelength of 254nm. On ten minutes of run time, repaglinide was retention at 7.4min. The extraction efficiency 95% for repaglinide. The intra-day and inter-day precision was in the terms of %RSD less than 1.76%. The developed method was validated and proposed method is useful for pharmacokinetics studies.  Keywords: Anti-diabetics, HPLC,Methanol,Phosphate buffer, Repaglinide

scholarly journals Development and validation of reversed phase high performance liquid chromatography (RP-HPLC) for quantification of captopril in rabbit plasma

2020 ◽  
Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Rabbit Plasma ◽  
Rp Hplc ◽  
Relative Standard

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.

scholarly journals Bioanalytical Method Development and Validation for Determination of Sulfasalazine in Rabbit Plasma by HPLC-UV

2021 ◽  
Vol 33 (7) ◽  
pp. 1692-1698
Author(s):  
S.S. Jadiya ◽  
N. Upmanyu ◽  
S. Arulmozhi ◽  
V. Jain ◽  
S. Sankaran ◽  
...  
Keyword(s):  
High Performance ◽  
Method Development ◽  
High Efficiency ◽  
Internal Standard ◽  
Ultra Violet ◽  
Precipitation Method ◽  
Pharmacokinetic Studies ◽  
Rabbit Plasma ◽  
Bioanalytical Method

In present study, an advanced, simple and a rapid reverse phase high performance liquid chromatography (RP-HPLC) method was developed for the quantitative determination of sulfasalazine in rabbit plasma. Sulfasalazine was separated using Chromatopak C-18 basic peerless (250 mm × 4.6 mm, 5μ) column in an isocratic mode using mobile phase consisting of the mixture of 10mM Ammonium acetate pH adjusted to 4.5 and acetonitrile (70:30 v/v) with a flow rate of about 1.0 mL/min at ambient temperature. An ultra-violet detection of sulfasalazine and the internal standard was carried out at 362 nm. Both sulfasalazine and internal standard (IS, 4-hydroxy benzoate) were extracted from plasma matrices with high efficiency using a simple protein precipitation method. The method was found to be highly selective with no carryover effects. Linearity of sulfasalazine was found with the range of 2.5-100 μg/mL with the value of r2 > 0.995 a correlation coefficient. At all three quality control levels, developed bioanalytical method was found as repeatable and reproducible as well. The average recoveries of sulfasalazine from plasma were in the range of 95.59-97.16%. The bioanalytical samples showed good and acceptable stability of sulfasalazine solution at different storage, packaging and handling conditions. Hence, in conclusion, the validated and developed HPLC-UV method could be effectively utilized for determination of sulfasalazine in pharmacokinetic studies involving novel formulations.

scholarly journals Extraction of Honey Polyphenols: Method Development and Evidence of Cis Isomerization ubertas Academica

2016 ◽  
Vol 11 ◽  
pp. ACI.S39739 ◽  
Author(s):  
Thibaut Istasse ◽  
Nicolas Jacquet ◽  
Thomas Berchem ◽  
Eric Haubruge ◽  
Bach Kim Nguyen ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Phenolic Acids ◽  
Extraction Method ◽  
High Performance ◽  
Method Development ◽  
Solid Phase ◽  
Phase Extraction ◽  
Minor Components ◽  
Coumaric Acid ◽  
Wild Carrot

Honey polyphenols have been studied with the objective of relating honeys to their floral sources. Initially synthesized by plant, these polyphenols can be found in the plant's nectar, which are collected by bees, which convert the nectar into honey. Consequently, polyphenols constitute minor components of honey. The development of a solid-phase extraction method for honey polyphenols is presented in this study. The technique employs Amberlite XAD-2 adsorbent and was tested on monofloral honeys from six different plants: acacia, chestnut, eucalyptus, thyme, sunflower, and wild carrot. Analyses were performed using high-performance liquid chromatography coupled with UV detection and mass spectrometry. Several phenolic acids and flavonoids were identified: caffeic and p-coumaric acids, quercetin, kaempferol, naringenin, chrysin, and pinocembrin. Generally, the quantity of a given polyphenol in the honey was around 0.2 mg/100 g of honey, except for chestnut honey, which contained around 3.0 mg of p-coumaric acid/100 g of honey. Analyses highlighted significant formation of cis isomers for phenolic acids during the extraction despite protection from light.

scholarly journals Method Development and Validation for Quantification of Potential Genotoxic Impurity, PyCl in Lansoprazole Hydrochloride using Liquid Chromatography Combined with Mass Spectrometry

2021 ◽  
Vol 33 (5) ◽  
pp. 1165-1168
Author(s):  
C. Purushotham Reddy ◽  
G. Venkateswara Rao ◽  
K. Ramakrishna ◽  
K.M.V. Narayana Rao
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Solution Stability ◽  
Selective Ion Monitoring ◽  
Acquity Uplc

A sensitive and robust high performance liquid chromatography combined with tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of potential genotoxic impurity (PGI), 2-(chloromethyl)-3-methyl-4-(2,2,2-trifluoroethoxy)-pyridine hydrochloride (PyCl) in lansoprazole as per ICH Q2 guideline. In this method, PyCl and lansoprazole were well-separated from each other on Acquity UPLC BEH-C18 column (50 × 4.6 mm × 1.7 μ) in a gradient elution mode with the mobile phase consisting of 0.1% formic acid in water (mobile phase-A) and acetonitrile (mobile phase-B) at a flow rate of 0.4 mL/min. For the quantitation of Py-Cl, selective ion monitoring (SIM) mode was used with m/z 240 ion in LC-MS method. The validated method was found to be precise, accurate and linear from the range of LOQ level to 150% with respect to sample concentration and the correlation co-efficient was found to be 0.998. Limit of detection (LOD) and limit of quantifications (LOQ) were found to be 0.000012 and 0.000004 mg/mL, respectively. The validated method was found to be sensitive and the recoveries were found to be well within the range from 83.4% to 95.9% for Py-Cl. Further, the solution stability was also established as the same were found to be stable upto 24 h.

scholarly journals RP-HPLC method development and validation for simultaneous estimation of efonidipine hydrochloride ethanolate and telmisartan in their synthetic mixture

2021 ◽  
pp. 190-195
Author(s):  
Grishma H Patel ◽  
Shreya D Adeshra ◽  
Dhananjay B Meshram
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Quality Control Laboratory ◽  
Efficient Option ◽  
Liquid Chromatographic

A Novel, selective, accurate and rapid Reversed Phase High Performance Liquid Chromatographic (RPHPLC) method for the analysis of Efonidipine Hydrochloride Ethanolate and Telmisartan in binary mixture has been developed and validated. The chromatographic system consisted of a Phenomenex Kinetex ® 5µ C18 Size: 150 * 4.6mm column and the separation was achieved by using ambient temperature with a mobile phase containing mobile Phase Acetonitrile:25mM Phosphate Buffer pH 4.9 (45:55). The samples were monitored at 253 nm for detection at a flow rate of 1.0 mL/min and the retention time was about 7.77 and 4.10 mins for Efonidipine Hydrochloride Ehanolate and Telmisartan respectively. The calibration curve was linear over the concentration range 5-30 and 10-60 ?g/mL for Efonidipine Hydrochloride Ehanolate and Telmisartan respectively. The proposed method is accurate in the range of 99.75% - 100.10% recovery and precise (%RSD of intraday variation and % RSD of inter day variation were found to be within the acceptance criteria). Therefore, this method can be used as a more convenient and efficient option for the analysis of Efonidipine Hydrochloride Ehanolate and Telmisartan in Quality control laboratory.

scholarly journals DEVELOPMENT OF A HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR ANALYZING DISODIUM 5′-GUANYLATE AND DISODIUM 5′-INOSINATE LEVELS IN FLAVOR ENHANCERS

2018 ◽  
Vol 10 (1) ◽  
pp. 133
Author(s):  
Dwi Karina Natalia ◽  
Harmita . ◽  
Taufiq Indra Rukmana
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
High Performance ◽  
Potassium Phosphate ◽  
Array Detector ◽  
Potassium Phosphate Buffer ◽  
Chromatography Method

Objective: This study aimed to develop a selective analytical method for assessing disodium 5′-guanylate and disodium 5′-inosinate levels in flavorenhancers.Methods: The levels were assessed using high-performance liquid chromatography (HPLC) with a photodiode array detector (PDA) (wavelength=255 nm) and a SunFire® C18 column (250 mm × 4.6 mm × 5 μm). The mobile phase comprised a mixture of potassium phosphate buffer and anion pair reagent-hexane-1-sulfonic acid sodium salt - with a flow rate of 1.2 mL/min. The ion pair was used to generate a neutral equilibrium, whichresulted in increased retention of the analytes. Optimized analysis conditions were then validated regarding accuracy, precision, linearity, selectivity,and the limits of detection and quantification.Results: The average levels of disodium 5′-inosinate in the six analyzed samples were 0.24±1.46, 0.21±2.69, 0.58±3.26, 0.21±0.84, 0.22±3.59, and0.47±2.21%, respectively. Regarding disodium 5′-guanylate, the average levels were 0.15±2.85, 0.15±0.12, 0.41±3.80, 0.16±1.72, 0.27±1.18, and0.34±1.83, respectively.Conclusion: The optimal conditions for analyzing disodium 5′-guanylate and disodium 5′-inosinateusing HPLC with a PDA and SunFire C18 columnwere λ=255 nm, a mobile phase of potassium phosphate buffer and sodium hexane sulfonate, and a flow rate of 1.2 mL/min. For disodium 5′-inosinate,its average levels in samples A–F were 0.24±1.46, 0.21±2.69, 0.58±3.26, 0.21±0.84, 0.22±3.59, and 0.47±2.21%, respectively. Meanwhile, the averagelevels of disodium 5′-guanylate in the samples were 0.15±2.85, 0.15±0.12, 0.41±3.80, 0.16±1.72, 0.27±1.18, and 0.34±1.83%, respectively.

Bioanalytical Method Development and Validation of Naproxen: Application to Bioequivalence Studies

2017 ◽  
Vol 8 (2) ◽  
Author(s):  
Senthil Rajan Dharmalingam ◽  
Srinivasan Ramamurthy ◽  
Sai Siddhardh ◽  
M. D. Basheerudhin
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Diclofenac Sodium ◽  
Pharmacokinetic Studies ◽  
Chromatography Method ◽  
Method Development And Validation ◽  
Liquid Chromatography Method ◽  
Development And Validation

A new selective and sensitive high-performance liquid chromatography method was developed for the quantification of Naproxen in human plasma using diclofenac sodium asinternal standard (IS). Chromatographic separation was achieved on aPhenomenex GEMINI C18 (150 x 4.6 mm, 5 mm) column. The mobile phase consists of a mixture of Acetonitrile: 0.5% Triethylamine buffer (50:50; v/v) and the pH of the mobile phase was adjusted to 3.5 by 85 % orthophosphoric acid. Flow rate of mobile phase was 1 mL/min.Detection was performed at 230nm. The calibration curve was linear over the concentration range from 10 to 120µg/mL. The detection (LOD) and quantification (LOQ) limits were 10 ng/mL and 25 ng/Ml respectively. The method was validated for accuracy, precision, specificity, robustness, and detection and quantification limits, in accordance with ICH guidelines.The developed method for the determination of Naproxen from human plasma has been found accurate, precise, selective, and suitable for the bioequivalence and pharmacokinetic studies.

scholarly journals Simultaneous Determination of Kynurenine and Kynurenic Acid by High-Performance Liquid Chromatography Photoirradiation System Using a Mobile Phase Containing 18-crown-6

2019 ◽  
Vol 12 ◽  
pp. 117864691983455
Author(s):  
Motomasa Atsumi ◽  
Ken-ichi Mawatari ◽  
Akari Morooka ◽  
Makoto Yasuda ◽  
Tomoko Fukuuchi ◽  
...  
Keyword(s):  
Hydrogen Peroxide ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
High Performance ◽  
Kynurenic Acid ◽  
Fluorometric Determination ◽  
The Mean

A high-performance liquid chromatography (HPLC) system has been developed for the fluorometric determination of kynurenine (KYN) and kynurenic acid (KYNA) in human serum using a mobile phase containing 18-crown-6. A retention time of KYNA was adjusted with pH of phosphate buffer in 18-crown-6. KYN and KYNA were separated on a CAPCELLPAK C18 (250 × 4.6 mm i.d.). The mobile phase consisted of 35 mmol/L phosphate buffer (pH 8.0)/methanol (85/15, v/v) containing 35 mmol/L hydrogen peroxide and 10 mmol/L 18-crown-6. The retention times of KYN and KYNA were 18and 24 minutes, respectively. The calibration graphs of KYN and KYNA were linear over the range 180 to 2900 and 1 to 84 nmol/L by injecting a 50-μL volume of KYN and KYNA, respectively. Pretreatment of serum was achieved by deproteinization only. The mean recoveries of KYN and KYNA from serum were more than 97%.

scholarly journals ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR LIMIT OF N-NITROSODIMETHYLAMINE BY LC-MS/MS OF EMPAGLIFLOZIN, LINAGLIPTIN AND METFORMIN HCL EXTENDED-RELEASE TABLETS

2021 ◽  
Vol 10 (5) ◽  
pp. 3534-3537
Author(s):  
Narayan Shrivas
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Extended Release ◽  
Method Development ◽  
Atmospheric Pressure Chemical Ionization ◽  
Pharmaceutical Research ◽  
Metformin Hydrochloride ◽  
Technical Requirement ◽  
Buffer Solution ◽  
Liquid Chromatography Tandem Mass

As a result of the devotion of The Limit of N-Nitrosodimethylamine (NDMA), a rapid and selective LC/MS/MS technique was created and validated for Empagliflozin, Linagliptin, and Metformin Hydrochloride Extended-Release Tablets. The ionization mode of Atmospheric pressure chemical ionization (APCI) was used with high-performance liquid chromatography-tandem mass spectrophotometry (LC-MS/MS). Separation of N-Nitrosodimethylamine (NDMA) was performed on Inertsil ODS-4 (250 mm X 4.6 mm), 5μm column with a run time of 40 minutes. A mixture of Methanol and Buffer solution (630 mg of ammonium format into 1000 mL of purified water) in the ratio of (10:90, v/v) was used as the mobile phase A. A mixture of acetonitrile and methanol comprised the mobile phase B in the ratio of (50:50) % v/v. Analytes were extracted from Empagliflozin, Linagliptin, and Metformin Hydrochloride Extended-Release Tablets. According to the International council for Harmonization of technical requirement for Pharmaceuticals for Human Uses (ICH) standards, the accuracy, precision, selectivity, recovery, and stability of the method have been validated. Over a concentration range of 0.4 -3.6 ng/mL, the technique exhibited linearity. for N- Nitrosodimethylamine of Empagliflozin, Linagliptin, and Metformin Hydrochloride Extended-Release Tablets with an acceptable correlation coefficient applies (1/X2) linear regression with weights A pharmaceutical study can benefit from this method because it is simple, fast, precise, and accurate, making it ideal for pharmaceutical research.

scholarly journals BIO-ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF AVELUMAB, AXITINIB AND ITS APPLICATION TO PHARMACOKINETIC STUDIES IN RABBIT PLASMA BY USING LCMS/MS

2021 ◽  
pp. 198-204
Author(s):  
SYED RAFI ◽  
KANTIPUDI RAMBABU
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Internal Standard ◽  
Pharmacokinetic Studies ◽  
Rabbit Plasma ◽  
System Suitability ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Stability Results ◽  
Good Agreement

Objective: An easy, quick, precise, active and reproducible LC-MS/MS technique was developed for the bioanalytical method of Avelumab and Axitinib using Cytarabine as an internal standard. Methods: This article summarizes the recent progress on bioanalytical LC-MS/MS methods using waters x-bridge phenyl column (150x4.6 mm, 3.5µ) column and organic mobile phase of 0.1% Tri fluoro acetic acid and Acetonitrile in 50:50 ratio. Results: The calibration curve was linear in the range of 2-40 ng/ml for avelumab and 0.5-10 ng/ml axitnib. Accuracy, precision, recovery, matrix effect and stability results were found to be within the suitable limits. Simple and efficient method was developed and utilized in pharmacokinetic studies to see the investigated analyte in body fluids. Conclusion: The application denotes all the parameters of system suitability, specificity, linearity and accuracy are in good agreement with USFDA guidelines and applied effectively for the investigation of pharmacokinetic studies in rabbit.

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