scholarly journals Development and Validation of a HPLC Method to Determine Griseofulvin in Rat Plasma: Application to Pharmacokinetic Studies

2008 ◽  
Vol 3 ◽  
pp. ACI.S953 ◽  
Author(s):  
Bo Wei ◽  
Dong Liang ◽  
Theodore R. Bates
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Rat Plasma ◽  
Hplc Method ◽  
Pharmacokinetic Studies ◽  
Dihydrogen Phosphate ◽  
Sodium Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Sodium Dihydrogen

A simple, specific, sensitive, and rapid high performance liquid chromatography (HPLC) method for the determination of griseofulvin in small volumes of rat plasma was developed and validated using warfarin as an internal standard. Biological sample preparation involved simple extraction with acetonitrile, followed by dilution with aqueous mobile phase buffer (20 mM sodium dihydrogen phosphate, pH 3.5) to eliminate any chromatographic solvent effects. Griseofulvin and warfarin were baseline separated and quantitated on a C18 reversed phase column (4.6 x 150 mm, 3.5 µm), using a mobile phase composed of a 20 mM aqueous solution of sodium dihydrogen phosphate-acetonitrile (55:45, v/v, pH 3.5) delivered at a flow rate of 1.0 mL/min, and with fluorescence detection (λexcitation = 300 nm, λemission = 418 nm). The method was proven to be linear over a plasma griseofulvin concentration range of 10 to 2500 ng/mL with a mean correlation coefficient of 0.9996. The intra-day and inter-day accuracy (relative error) were in the range of 0.89% to 9.26% and 0.71% to 7.68%, respectively. The within-day precision (coefficient of variation) was less than 3.0% and the between-day precision was less than 7.5%. The mean recovery of griseofulvin from rat plasma was found to be 99.2%. The limit of detection (LOD) and the limit of quantification (LOQ) of griseofulvin were determined to be 1 ng/mL and 10 ng/mL, respectively. The developed method was successfully applied to quantitatively assess the pharmacokinetics of griseofulvin in rats following a single 50 mg/kg oral dose of the drug.

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 Validated RP-HPLC Method for the Assay of Etoricoxib (A Non-Steroidal Anti-Inflammatory Drug) in Pharmaceutical Dosage Forms

2012 ◽  
Vol 9 (2) ◽  
pp. 832-838 ◽  
Author(s):  
Srinivasu Topalli ◽  
T. G. Chandrashekhar ◽  
M. Mathrusri Annapurna
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms

A simple, accurate, sensitive and reproducible reverse phase high performance liquid chromatographic method has been developed for the quantitative determination of Etoricoxib in pharmaceutical dosage forms. The assay was performed on Hypersil ODS C-18 (250 x 4.6 mm., 5µm particle size) column using acetonitrile and potassium dihydrogen phosphate buffer (pH 4.2) (46:54 % v/v) as mobile phase with UV detection at 280 nm (flow rate 1.2 ml/min). Bromhexine was used as an internal standard. Quantization was achieved by measurement of the peak area ratio of the drug to the internal standard. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.0704 µg ml-1and 0.2134 µg ml-1respectively. Each analysis required no longer than 10 minutes. The calibration curve was linear over the concentration range from 0.5-85.0 µg ml-1. The retention times of Etoricoxib and Bromhexine were found to be 3.083 and 7.631 minutes respectively. The proposed method was validated according to the ICH guidelines and can be used successfully to analyse marketed formulations.

scholarly journals Development and Validation of Bioanalytical HPLC Method For Estimation of Telmisartan In Rat Plasma: Application To Pharmacokinetic Studies

2013 ◽  
Vol 11 (2) ◽  
pp. 121-127 ◽  
Author(s):  
Jaydeep M Patel ◽  
Anjali P Dhingani ◽  
Kevin C Garala ◽  
Mihir K Raval ◽  
Navin R Sheth
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Rat Plasma ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmacokinetic Parameters ◽  
Pharmacokinetic Studies ◽  
Limit Of Quantification ◽  
Liquid Chromatographic

A simple, specific, sensitive and rapid reversed phase high performance liquid chromatographic (HPLC) method has been developed and validated for the determination of telmisartan in small volumes of rat plasma. Biological sample preparation involving simple extraction with organic solvent, followed by dilution with mobile phase was adopted to eliminate any chromatographic solvent effects. The method was proven to be linear over a plasma concentration range of 10 to 1000 ng/mL with a mean correlation coefficient of 0.9942. The limit of detection and the limit of quantification of the newly developed method were determined to be 1 ng/mL and 10 ng/mL, respectively. The method was successfully applied to assess pharmacokinetic parameters of telmisartan in Wister rats following a single oral dose (1.8 mg/kg, b.w.). The developed method was established as a rapid analytical tool in a pharmacokinetic study as it required short retention time, high precision, sensitivity and small volumes of plasma for analysis. DOI: http://dx.doi.org/10.3329/dujps.v11i2.14562 Dhaka Univ. J. Pharm. Sci. 11(2): 121-127, 2012 (December)

scholarly journals A sensitive HPLC-FLD method for the quantification of 6-O-demethylmenisporphine isolated from Menispermi Rhizoma in rat plasma

2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Jinxia Wei ◽  
Jia Shao ◽  
Yanan Li ◽  
Yubo Li
Keyword(s):  
Mobile Phase ◽  
Internal Standard ◽  
Rat Plasma ◽  
Hplc Assay ◽  
Isocratic Elution ◽  
Fluorescence Detector ◽  
Limit Of Quantification ◽  
The Mean ◽  
Preclinical Safety ◽  
Concentration Levels

Abstract Background To investigate the pharmacokinetics of 6-O-demethylmenisporphine, an oxoisoaporphine alkaloid with significant anti-tumor activities and isolated from Menispermi Rhizoma, a novel and sensitive HPLC assay was established for 6-O-demethylmenisporphine quantification in rat plasma. Methods Peak responses were detected by a highly selective and sensitive fluorescence detector with 426-nm excitation and 514-nm emission wavelengths. Curcumin was employed as the internal standard (IS). A Capcell Pak C18 column (150 mm × 4.6 mm i.d., 5 μm) and an isocratic elution procedure with a flow rate of 1.0 mL/min were used to exclude the endogenous interfering substance. Acetonitrile-water (68:32, v/v) containing 1% formic acid was employed as mobile phase. A 7-point calibration curve that covered the concentration range of 10–2500 ng/mL was constructed. Results A good linearity was observed with a correlation coefficient (r) of 0.9993. The lower limit of quantification for 6-O-demethylmenisporphine was 10 ng/mL. The mean recoveries of analyte in rat plasma exceeded 80.5%. The precision at four concentration levels was within 11.3% and the accuracy ranged from − 7.6 to 6.7%. Conclusion Using this new HPLC-FLD method, the investigation of plasma samples from rats following oral dosing of neat compound and Menispermi Rhizoma extract was successfully conducted. The results will provide a reference for the evaluation of preclinical safety of 6-O-demethylmenisporphine.

scholarly journals Photostability study of amlodipine besylate tablets packed in primary packaging

2021 ◽  
Vol 10 (1) ◽  
pp. 20-28
Author(s):  
Ivana Savić-Gajić ◽  
Ivan Savić ◽  
Predrag Sibinović ◽  
Valentina Marinković
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Coefficient Of Determination ◽  
Amlodipine Besylate ◽  
Limit Of Quantification ◽  
First Order Kinetics ◽  
The Given

In this study, the modified stability-indicating RP-HPLC method was validated for quantitative analysis of amlodipine besylate in the presence of its impurity D (3-ethyl 5-methyl 2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-6-methylpyridine-3,5-dicarboxylate). The method was applied for the determination of an analyte in the tablets and irradiated samples packed in the primary packaging (Alu/PVC/PVDC blister packaging). The efficient chromatographic separation was achieved using a ZORBAX Eclipse XDB-C18 column (4.6×250 mm, 5 mm) with isocratic elution of mobile phase which consisted of acetonitrile:methanol:triethylamine solution (15:35:50, v/v/v) (pH 3.0). The flow rate of the mobile phase was 1 mL min-1, while the detection of amlodipine besylate was carried out at 273 nm. Amlodipine besylate and its impurity D were identified at the retention times of 16.529 min and 2.575 min, respectively. The linearity of the method with the coefficient of determination of 0.999 was confirmed in the concentration range of 10 - 75 µg mL-1 for amlodipine besylate. The limit of detection was 0.2 µg mL-1, while the limit of quantification was 0.66 µg mL-1. After UV and Vis radiation of the tablets packed in the primary packaging, the content of amlodipine besylate was reduced by 22.38% and 19.89%, respectively. The presence of new degradation products was not detected under the given chromatographic conditions. The photodegradation of amlodipine besylate followed pseudo-first-order kinetics. Based on the half-life of amlodipine besylate (38.4 days for UV radiation and 43.3 days for Vis radiation), it was concluded that amlodipine besylate in the tablets has satisfactory photostability after its packing in the Alu/PVC/PVDC blister packaging.

scholarly journals LC-MS characterization of acid degradation products of metoclopramide: Development and validation of a stability-indicating RP-HPLC method

2020 ◽  
Vol 11 (1) ◽  
pp. 781-789
Author(s):  
Sriram Valavala ◽  
Nareshvarma Seelam ◽  
Subbaiah Tondepu ◽  
Suresh Kandagatla
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Hplc Technique

The present study aims to develop a simple, accurate and specific stability-indicating RP-HPLC technique for the analysis of metoclopramide in the presence of its stress degradation products and characterization of degradation compounds by LC-MS/MS analysis. As per ICH Q1A-R2 guidelines, the drug was exposed to acid hydrolytic stress condition. Three degradation products were formed for MCP in acid hydrolysis. The liquid chromatography was processed on a Luna C18-(2) 100A,250×4.6mm 5micron column using an isocratic mobile phase consisting of 0.1% formic acid in water-acetonitrile (20:80, v/v) by adjusting the mobile phase at 1 ml/min flow rate with wavelength detection at 273 nm. The developed procedure was applied to LC-MS/MS (liquid chromatography-tandem mass spectrometry) for the characterization of all the degradant components. Total new three degradation compounds were recognized and identified by LC-MS/MS. The developed RP-HPLC technique was validated as per the ICH Q2-R1 guidelines. Limit of detection and limit of quantification values of MCP were evaluated from the linearity graph and were found to be 5.23 µg/ml and 17.44 µg/ml. Accuracy study was established at 80.0, 100.0 and 120.0 µg/ml concentration levels and the findings were found in the range of 98.4% - 101.8%. The linearity of the technique was assessed over the drug concentration range of 50.0 µg/ml to 250.0 µg/ml and the regression equation, slope and correlation coefficient values were found to be y = 10618x + 1623.2, 10618 and 0.9996 respectively. The developed technique was uninterruptedly applied for the quantification of metoclopramide inactive pharmaceuticals.

scholarly journals OFAT versus DOE as two optimization protocols for the chromatographic analysis of some OTC pharmaceuticals carrying negative cardiovascular effects and administered by pregnant and breast-feeding females: Application to dose dependent effect

2020 ◽  
pp. 1-14
Author(s):  
Dina El Sherbiny ◽  
Mary E. K. Wahba
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Cardiovascular Effects ◽  
Dihydrogen Phosphate ◽  
Sodium Dihydrogen Phosphate ◽  
Pregnancy And Lactation ◽  
Face Centered ◽  
Comparison Of The Results ◽  
Sodium Dihydrogen

Abstract A simple HPLC technique has been utilized for rapid and sensitive quantitative analysis of two mixtures of drugs that are used during pregnancy and lactation. Drugs of the first mixture are used to manage gastrointestinal tract illness that are common during early stages of pregnancy, while pharmaceutical agents of the second mixture are administered over the counter as galactagogues or to overcome postpartum depression. Mixture I includes famotidine (FMT), ranitidine (RNT), nizatidine (NZT), and pantoprazole (PNT), which were separated on a C18 column using a mobile phase composed of methanol: 0.02 M sodium dihydrogen phosphate (60:40, v/v) of pH 6.9, adopting UV detection at 240 nm at a flow rate of 1 mL/min. Mixture II on the other hand, consists of domperidone (DOM), metoclopramide (MET), and sulpiride (SUL). These drugs were eluted using the same column and flow rate as those in mixture I, using a mobile phase consisting of acetonitrile: 0.075 M sodium dihydrogen phosphate (30:70, v/v) of pH 6 adopting a detection wavelength 270 nm. Two optimization protocols were utilized to optimize the chromatographic separation conditions, namely one factor at a time (OFAT) and design of experiments (DOE) where face centered cube response surface experimental design was chosen for this investigation. Comparison of the results obtained from both protocols reveals the accordance between them. Full validation procedure under guidance of United States Pharmacopoeia (USP) was applied to the proposed methods which enabled their application to separate the drugs of both mixtures in spiked rat whole blood samples and in vivo analysis of rat heart blood.

A NOVEL HPLC METHOD FOR ESTIMATION OF GENOTOXIC IMPURITY 3-ACETAMIDOBENZENE 1, 2 DICARBOXYLIC ACID IN KEY STARTING MATERIAL 3-ACETAMIDOPTHALIC ANHYDRIDE OF APREMILAST API

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (05) ◽  
pp. 42-46
Author(s):  
P. Shinde ◽  
◽  
S. Shirke ◽  
R. Dwivedi ◽  
U Dhuppad
Keyword(s):  
Dicarboxylic Acid ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Research Work ◽  
Hplc Method ◽  
Starting Material ◽  
Phase Method ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Normal Phase Hplc

3-Acetamidobenzene -1, 2-dicarboxylic acid is a potential genotoxic impurity which gets formed during synthesis of 3- acetamidopthalic anhydride, a Key Starting Material (KSM) for manufacturing of apremilast API. During handling upon exposure to moisture, the anhydride ring of KSM 3-acetamidopthalic anhydride opens to form the acid. Hence Reverse phase HPLC method is not a feasible and robust option for estimation of this impurity. To overcome these problems a normal phase HPLC method is developed and proposed in this research work. Immobilized Chiral pack IA column from Daicel is used for estimation. n-Hexane and isopropyl alcohol in 90:10 (v/v) ratio modified with 0.1% trifluroacetic acid is used as mobile phase. Method is validated as per ICH guidelines. Limit of Detection (LOD) and Limit of Quantification (LOQ) are found to be 0.47 ppm (0.0047%) and 1.42 ppm (0.0142%), respectively. The method is linear over LOQ to 150%. Recovery is within limits (80-120%). Method is robust for parameters like mobile phase composition, flow rate, wavelength changes and column oven temperature.

scholarly journals Bioanalytical LC-MS/MS method for Determination and comparison of Selexipag Assay in various Biological materials and its Application to Pharmacokinetics Studies in Rat plasma

2020 ◽  
Vol 11 (2) ◽  
pp. 2210-2220
Author(s):  
Namburi LA Amara babu ◽  
Kalyani Koganti ◽  
Babji Palakeeti ◽  
Koduri SV Srinivas ◽  
Koya Prabhakara Rao
Keyword(s):  
Internal Standard ◽  
Biological Materials ◽  
Rat Plasma ◽  
Pharmacokinetic Studies ◽  
Liquid Chromatography Mass Spectrometry ◽  
Rabbit Plasma ◽  
Limit Of Quantification ◽  
Mass Detector ◽  
Regression Correlation ◽  
Lower Medium

A rapid, sensitive and selective bioanalytical method was developed and validated by Liquid Chromatography - Mass spectrometry (LC-MS/MS) for determination and comparison of Selexipag% assay in various biological materials. Selexipag wasextractedand compared its % assay after protein precipitation technique from various biological materials such as rat plasma, rabbit plasma, human plasma and urine. Ambrisentan was selected as internal standard. Selected analytical column Waters, X-Bridge C18 3.5µ (50 x 4.6 mm), mobile phase consists of Hexane sulfonic acid and Acetonitrile (80:20 v/v) at a flow rate of 1.0 mL /minin isocratic modeand Selexipag was determined by the +ve mode of electrospray ionization by using Mass detector. The method was developed to assess the lowerlimit of detection (LLOD)(0.5 ng/mL), lower limit of quantification(LLOQ) (5 ng/mL) concentrations and Linearity range of 1 ng/mL to 20 ng/mLconcentration with regression correlation coefficient 0.999 were observed for Selexipag in Rat plasma. The test samples at lower, medium and higher concentrationsof Selexipag shows precision (% CV was 0.8 to 1.11) and accuracy results (97.3 % to 100.6%) for inter-day and intra-day analysis at0.5, 5, 10, 15 ng/mL concentrationsof Selexipag. Appreciable recoveries for Selexipag were observed when extracted in Rat plasma compared with other biological materials. Stability of Selexipag exists in all conditions like wet extract, bench top, freeze-thaw and in instrument auto sampler as per FDA guidelines. This method indicates good results of accuracy, precision, linearity, recovery, stability and pharmacokinetic studies in rat plasma for clinical trials.

scholarly journals Developement of Quantitative Analysis of Sparfloxacin by High Performance Liquid Chromatography

1970 ◽  
Vol 6 (1) ◽  
pp. 21-23
Author(s):  
Narun Nahar Rahman ◽  
Shahabuddin Ahmad
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Sodium Dihydrogen Phosphate ◽  
Buffer Solution ◽  
Tablet Dosage ◽  
Liquid Chromatographic ◽  
Sodium Dihydrogen

An attempt has been made to develop a simple, sensitive and rapid high performance liquid chromatographic (HPLC) method of analysis for sparfloxacin using 35% acetonitrile in buffer solution as mobile phase. Buffer solution (40 mM of sodium dihydrogen phosphate in de-ionized water) was used as solvent to dissolve sparfloxacin and 0.05mg/ml stock solution was prepared. Sparfloxacin solution was scanned with UV-spectrophotometer and the absorption maximum (λmax) was found at 292 rim. This method was successfully applied to four tablet dosage forms of sparfloxacin encoded as ?, ?, ?, and ?, from four different companies and the result was found to be satisfactory and reproducible. Key words: Sparfloxacin, HPLC, analysis Dhaka Univ. J. Pharm. Sci. 6(1): 21-23, 2007 (June) The full text is of this article is available at the Dhaka Univ. J. Pharm. Sci. website

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