Stability-Indicating Assay for the Determination of Pentobarbital Sodium in Liquid Formulations

A stability-indicating assay by reversed-phase high performance liquid chromatography (RP-HPLC) method was developed for the determination of pentobarbital sodium in oral formulations: a drug used for infant sedation in computed tomography (CT) or magnetic resonance imaging (MRI) scan. The chromatographic separation was achieved on a reversed-phase C18 column, using isocratic elution and a detector set at 214 nm. The optimized mobile phase consisted of a 0.01 M potassium buffer pH 3 and methanol (40 : 60, v/v). The flow rate was 1.0 mL/min and the run time of analysis was 5 min. The linearity of the method was demonstrated in the range of 5 to 250 μg/mL pentobarbital sodium solution (r2= 0.999). The limit of detection and limit of quantification were 2.10 and 3.97 μg/mL, respectively. The intraday and interday precisions were less than 2.1%. Accuracy of the method ranged from 99.2 to 101.3%. Stability studies indicate that the drug is stable to sunlight and in aqueous solution. Accelerated pentobarbital sodium breakdown by strong alkaline, acidic, or oxidative stress produced noninterfering peaks. This method allows accurate and reliable determination of pentobarbital sodium for drug stability assay in pharmaceutical studies.

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A SIMPLE (HPLC–UV) METHOD FOR THE QUANTIFICATION OF COLCHICINE IN BULK AND ETHOSOMAL GEL NANO-FORMULATION AND ITS VALIDATION

International Journal of Pharmacy and Pharmaceutical Sciences ◽

10.22159/ijpps.2017v9i7.18336 ◽

2017 ◽

Vol 9 (7) ◽

pp. 72 ◽

Cited By ~ 1

Author(s):

Ibrahim M. Abdulbaqi ◽

Yusrida Darwis ◽

Nurzalina Abdul Karim Khan ◽

Reem Abou Assi ◽

Gabriel Onn Kit Loh

Keyword(s):

High Performance ◽

Limit Of Detection ◽

Degradation Products ◽

Reversed Phase ◽

Hplc Method ◽

Acid Oxidation ◽

Limit Of Quantification ◽

Stability Indicating ◽

Stress Degradation

Objective: To develop and validate a stability-indicating reversed phase high-performance liquid chromatography (RP-HPLC) method for the determination of colchicine in bulk and ethosomal gel nano-formulation.Methods: The chromatographic conditions were optimized using stainless steel Hypersil Gold C-18 analytical column with the dimensions of 250 mm x 4.6 mm ID x 5 µm. The mobile phase consisted of acetonitrile and ammonium acetate buffer (20 mmol/l, pH=4.85) in the ratio of 32:68 v/v. The ﬂow rate was set at 1 ml/min and the detection wavelength was 353 nm. The column was maintained at 30 °C and the injection volume was 10 µl. The stability of colchicine in different conditions was investigated by exposing the drug to stress degradation using acid, base, oxidation, heat and light.Results: There was no interference from excipients, impurities, dissolution media or degradation products at the retention time of colchicine 5.9 min indicating the specificity of the method. The limit of detection (LOD) and the limit of quantification (LOQ) were 8.64 ng/ml and 26.17 ng/ml respectively. The drug showed good stability under heat, acid, oxidation and light, but substantial degradation was observed under alkali condition. The procedure was validated for specificity, linearity, accuracy and precision.Conclusion: A simple, rapid, specific and stability-indicating HPLC–UV method for the determination of colchicine in the pure and ethosomal gel was successfully developed. The developed method was statistically confirmed to be accurate, precise, and reproducible.

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Development and Validation of HPLC Method for Simultaneous Determination of Ceftriaxone and Cefaclor in Commercial Formulations and Biological Samples

Journal of the Mexican Chemical Society ◽

10.29356/jmcs.v57i4.195 ◽

2017 ◽

Vol 57 (4) ◽

Cited By ~ 2

Author(s):

Jasmin Shah ◽

M. Rasul Jan ◽

Sultan Shah ◽

M. Naeem Khan

Keyword(s):

Simultaneous Determination ◽

Human Plasma ◽

High Performance ◽

Limit Of Detection ◽

High Performance Liquid Chromatographic ◽

Reversed Phase ◽

Hplc Method ◽

Limit Of Quantification ◽

Spiked Human Plasma

A reversed phase high performance liquid chromatographic method has been developed for the simultaneous determination of cefaclor and ceftriaxone cephalosporin antibiotic. The developed method has been validated and applied to mixtures of the commercial formulation and spiked human plasma. A mediterranea C18 column (4.6 × 250 mm) was used with isocratic solvent delivery system and UV-visible detector. Different experimental parameters like solvent composition (acetonitrile: methanol: triethyl amine buffer 1:1:2 (v/v), flow rate of mobile phase (0.6 mLmin-1), pH of the buffer (7), and wavelength (260 nm) were optimized for effective separation and esolution of the analyte peaks. The separation was achieved in 6 min with retention times of 4.94 ± 0.056 min and 3.39 ± 0.022 min for cefaclor and ceftriaxone respectively. The linear range for both the studied drugs was found to be 0.5-250 μgmL-1 with r2 of 0.9987 (cefaclor) and 0.9997 (ceftriaxone). The limit of detection (3.3 σ/S) was found to be 2.34 × 10-2 μgmL−1 and 1.70 × 10−2 μgmL-1, respectively, for cefaclor and ceftriaxone. Similarly limit of quantification (10σ/S) was 7.10 × 10−2 μgmL-1 for cefaclor and 5.15 × 10−2 μgmL-1 for ceftriaxone. The chromatographic procedure was applied to commercial formulations and spiked human plasma and the results were compared with literature HPLC method.

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DEVELOPMENT OF VALIDATED RP-HPLC METHOD FOR THE QUANTITATIVE ANALYSIS OF CHROMIUM PICOLINATE III IN A DIET VINEGAR FORMULATION

INDIAN DRUGS ◽

10.53879/id.50.05.p0048 ◽

2013 ◽

Vol 50 (05) ◽

pp. 48-52

Author(s):

A Lodhi ◽

◽

A Jain ◽

B. Biswal

Keyword(s):

High Performance ◽

Limit Of Detection ◽

High Performance Liquid Chromatographic ◽

Reversed Phase ◽

Hplc Method ◽

Chromium Picolinate ◽

Limit Of Quantification ◽

Pharmaceutical Dosage Forms ◽

Liquid Chromatographic Method ◽

Liquid Chromatographic

A validated high performance liquid chromatographic method was developed for the determination of chromium picolinate in pharmaceutical dosage forms. The analysis was performed at room temperature using a reversed-phase ODS, 5µm (250×4.6) mm column. The mobile phase consisted of acetonitrile: buffer (60:40 V/V) at a flow rate of 0.5 mL/min. The PDA-detector was set at 264 nm. The developed method showed a good linear relationship in the concentration range from 1.5 – 12.5 µg/mL with a correlation coefficient from 0.999. The limit of detection and limit of quantification were 0.0540513 and 0.1637919 µg/mL respectively.

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Determination of tigecycline in turkey plasma by LC-MS/MS: validation and application in a pharmacokinetic study

Polish Journal of Veterinary Sciences ◽

10.1515/pjvs-2017-0029 ◽

2017 ◽

Vol 20 (2) ◽

pp. 241-249 ◽

Cited By ~ 2

Author(s):

A. Jasiecka-Mikołajczyk ◽

J.J. Jaroszewski

Keyword(s):

Pharmacokinetic Study ◽

High Performance ◽

Limit Of Detection ◽

Internal Standard ◽

Reversed Phase ◽

Selected Reaction Monitoring ◽

Limit Of Quantification ◽

Complicated Skin ◽

Intravenous And Oral Administration

Abstract Tigecycline (TIG), a novel glycylcycline antibiotic, plays an important role in the management of complicated skin and intra-abdominal infections. The available data lack any description of a method for determination of TIG in avian plasma. In our study, a selective, accurate and reversed-phase high performance liquid chromatography-tandem mass spectrometry method was developed for the determination of TIG in turkey plasma. Sample preparation was based on protein precipitation and liquid-liquid extraction using 1,2-dichloroethane. Chromatographic separation of TIG and minocycline (internal standard, IS) was achieved on an Atlantis T3 column (150 mm × 3.0 mm, 3.0 μm) using gradient elution. The selected reaction monitoring transitions were performed at 293.60 m/z → 257.10 m/z for TIG and 458.00 m/z → 441.20 m/z for IS. The developed method was validated in terms of specificity, selectivity, linearity, lowest limit of quantification, limit of detection, precision, accuracy, matrix effect, carry-over effect, extraction recovery and stability. All parameters of the method submitted to validation met the acceptance criteria. The assay was linear over the concentration range of 0.01-100 μg/ml. This validated method was successfully applied to a TIG pharmacokinetic study in turkey after intravenous and oral administration at a dose of 10 mg/kg at various time-points.

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Stability-Indicating HPLC Assay for Determination of Idebenone in Pharmaceutical Forms

Journal of Analytical Methods in Chemistry ◽

10.1155/2015/835986 ◽

2015 ◽

Vol 2015 ◽

pp. 1-5 ◽

Cited By ~ 2

Author(s):

Sonoube Kombath ◽

Issa-Bella Balde ◽

Sandra Carret ◽

Sofiane Kabiche ◽

Salvatore Cisternino ◽

...

Keyword(s):

Mobile Phase ◽

Drug Stability ◽

Reversed Phase ◽

Hplc Assay ◽

Reliable Determination ◽

Stability Indicating ◽

Chromatography Analysis ◽

Stability Indicating Method ◽

Detection And Quantification

A stability-indicating method was validated for the determination in pharmaceutical forms of idebenone a coenzyme Q10-like compound. The assay was achieved by liquid chromatography analysis using a reversed-phase C18 column and a detector set at 480 nm. The optimized mobile phase consisted of isocratic flow rate at 1.0 mL/min for 3 min with methanol. The linearity of the assay was demonstrated in the range of 3.0 to 8.0 mg/mL with a correlation coefficientr2>0.998. The limits of detection and quantification were 0.03 and 0.05 mg/mL, respectively. The intraday and interday precisions were less than 1.0%. Accuracy of the method ranged from 98.6 to 101.5% with RSD < 0.6%. Specificity of the assay showed no interference from tablets components and breakdown products formed by alkaline, acidic, oxidative, sunlight, and high temperature conditions. This method allows accurate and reliable determination of idebenone for drug stability assay in pharmaceutical studies.

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Development and Validation of an RP-HPLC Method for CB13 Evaluation in Several PLGA Nanoparticle Systems

The Scientific World JOURNAL ◽

10.1100/2012/737526 ◽

2012 ◽

Vol 2012 ◽

pp. 1-9 ◽

Cited By ~ 3

Author(s):

J. Álvarez-Fuentes ◽

L. Martín-Banderas ◽

I. Muñoz-Rubio ◽

M. A. Holgado ◽

M. Fernández-Arévalo

Keyword(s):

Size Distribution ◽

High Performance ◽

Limit Of Detection ◽

High Performance Liquid Chromatographic ◽

Plga Nanoparticles ◽

Reversed Phase ◽

Hplc Method ◽

Array Detector ◽

Limit Of Quantification ◽

Rp Hplc

A simple, fast, and reversed-phase high-performance liquid chromatographic (RP-HPLC) method has been developed and validated for determining of a cannabinoid derivate, which displays potent antihyperalgesic activity, 1-naphthalenyl[4-(pentyloxy)-1-naphthalenyl]methanone (CB13) into PLGA nanoparticles. Separation was achieved in a C18 column using a mobile phase consisting of two solvents: solvent A, consisting of acetonitrile : water : acetic acid (75 : 23.7 : 1.3 v/v), and solvent B, consisting of acetonitrile. An isocratic method (70 : 30 v/v), with a flow rate of 1.000 mL/min, and a diode array detector were used. The developed method was precise, accurate, and linear over the concentration range of analysis with a limit of detection and a limit of quantification of 0.5 and 1.25 μg/mL, respectively. The developed method was applied to the analysis of CB13 in nanoparticles samples obtained by three different procedures (SEV, FF, and NPP) in terms of encapsulation efficiency and drug release. Nanoparticles size and size distribution were also evaluated founding that NPP method presented the most lowest particle sizes with narrow-size distribution (≈320 nm) and slightly negative zeta potential (≈−25 mV) which presumes a suitable procedure for the synthesis of PLGA-CB13 nanoparticles for oral administration.

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A Stability Indicating UPLC Method for the Determination of Tramadol Hydrochloride: Application to Pharmaceutical Analysis

Chromatography Research International ◽

10.1155/2012/870951 ◽

2012 ◽

Vol 2012 ◽

pp. 1-9 ◽

Cited By ~ 5

Author(s):

Kanakapura B. Vinay ◽

Hosakere D. Revanasiddappa ◽

Cijo M. Xavier ◽

Pavagada J. Ramesh ◽

Madihalli S. Raghu

Keyword(s):

Limit Of Detection ◽

Potassium Dihydrogen Phosphate ◽

Reversed Phase ◽

Forced Degradation ◽

Dihydrogen Phosphate ◽

Uv Detector ◽

Limit Of Quantification ◽

Tramadol Hydrochloride ◽

Stability Indicating

The use of Ultra Performance Liquid Chromatography (UPLC), with a rapid 5-minute reversed phase isocratic separation on a 1.7 μm reversed-phase packing material to provide rapid ‘‘high throughput’’ support for tramadol hydrochloride (TMH) is demonstrated. A simple, precise and accurate stability-indicating isocratic UPLC method was developed for the determination of TMH in bulk drug and in its tablets. The method was developed using Waters Aquity BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with mobile phase consisting of a mixture of potassium dihydrogen phosphate buffer of pH 2.8 and an equal volume of acetonitrile (60 : 40 v/v). The eluted compound was detected at 226 nm with a UV detector. The standard curve of mean peak area versus concentration showed an excellent linearity over a concentration range 0.5–300 μg mL−1 TMH with regression coefficient (r) value of 0.9999. The limit of detection (S/N =3) was 0.08 μg mL−1 and the limit of quantification (S/N =10) was 0.2 μg mL−1. Forced degradation of the bulk sample was conducted an accordance with the ICH guidelines. Acidic, basic, hydrolytic, oxidative, thermal and photolytic degradation were used to assess the stability indicating power of the method. TMH was found to degrade significantly in acidic, basic and oxidative stress conditions and stable in thermal, hydrolytic and photolytic conditions.

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HPLC method validation and application for organic acid analysis in wine after solid-phase extraction

Macedonian Journal of Chemistry and Chemical Engineering ◽

10.20450/mjcce.2016.1073 ◽

2016 ◽

Vol 35 (2) ◽

pp. 225 ◽

Cited By ~ 12

Author(s):

Violeta Ivanova-Petropulos ◽

Krste Tašev ◽

Marina Stefova

Keyword(s):

Solid Phase Extraction ◽

Organic Acids ◽

High Performance ◽

Limit Of Detection ◽

Solid Phase ◽

Hplc Method ◽

Phase Extraction ◽

Hplc Separation ◽

Limit Of Quantification

A solid-phase extraction method followed by reverse phase high-performance liquid chromatography (RP-HPLC) was optimized and validated for the quantitative determination of tartaric, malic, shikimic, lactic, citric and succinic acids in wine. Solid-phase extraction was carried out with C18 cartridges and extraction recoveries for all acids ranging from 98.3 to 103% were obtained. HPLC separation was performed with isocratic elution on a LiChrosorb RP-18 column (250 × 4.6 mm I.D., 5 µm) protected with the appropriate guard column. The mobile phase was a 5 mM solution of H3PO4 with pH 2.1 at a flow rate of 1 ml/min. Detection of the organic acids was performed at 210 nm. The developed method was validated by checking its linearity, limit of detection (LOD), limit of quantification (LOQ), precision and recovery. The method was applied to the analysis of organic acids in Macedonian red and white wines.

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STABILITY INDICATING RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS DETERMINATION OF VILDAGLIPTIN AND METFORMIN IN PHARMACEUTICAL DOSAGE FORM

International Journal of Pharmacy and Pharmaceutical Sciences ◽

10.22159/ijpps.2017v9i3.16233 ◽

2017 ◽

Vol 9 (3) ◽

pp. 150

Author(s):

Ramesh Jayaprakash ◽

Senthil Kumar Natesan

Keyword(s):

High Performance ◽

Method Development ◽

Limit Of Detection ◽

Potassium Dihydrogen Phosphate ◽

Hplc Method ◽

Dihydrogen Phosphate ◽

Pharmaceutical Dosage Form ◽

Stability Indicating ◽

Rp Hplc

Objective: The present study was aimed to develop a rapid, accurate, linear, sensitive and validate stability-indicating high performance liquid chromatographic [RP-HPLC] method for determination of vildagliptin and metformin in pharmaceutical dosage form.Methods: The chromatographic separation was performed on kromasil-C18 column [4.5 x 250 mm; 5 µm] using a mobile phase consisting of 0.05 mmol potassium dihydrogen phosphate buffer: acetonitrile [80:20 v/v], [pH adjusted to 3.5 using orthophosphoric acid]. The flow rate is 0.9 ml/min and the detection was carried out at 263 nm.Results: The chromatographic condition, the peak retention time of metformin and vildagliptin were found to be 2.215 min and 2.600 min respectively. Stress testing was performed in accordance with an international conference on harmonization [ICH] Q1A R2 guidelines. The method was validated as per ICH Q2 R1 guidelines. The calibration curve was found to be linear in the concentration range of 5-17.5 µg/ml and 50-175 µg/ml for vildagliptin and metformin. The limit of detection and quantification was found to be 0.0182 µg/ml and 0.0553 µg/ml for vildagliptin and 0.4451 µg/ml and 1.3490 µg/ml for metformin respectively.Conclusion: A new sensitive, simple and stability indicating reverse-phase high-performance liquid chromatography [RP-HPLC] method has been developed and validated for the determination of vildagliptin and metformin. The proposed method can be used for routine determination of vildagliptin and metformin.

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STABILITY INDICATING VALIDATED HPLC METHOD FOR THE DETERMINATION OF ZANUBRUTINIB IN BULK AND PHARMACEUTICAL DOSAGE FORM

Asian Journal of Pharmaceutical and Clinical Research ◽

10.22159/ajpcr.2020.v13i10.38621 ◽

2020 ◽

pp. 159-162

Author(s):

M. VIJAYA KUMARI ◽

CH. BALASEKHAR REDDY

Keyword(s):

High Performance ◽

Limit Of Detection ◽

Pharmaceutical Preparations ◽

Reversed Phase ◽

Hplc Method ◽

Limit Of Quantification ◽

Intermediate Precision ◽

Pharmaceutical Dosage Form ◽

Acceptable Limit ◽

Relative Standard

Objective: An accurate, rapid economical and straight forward, reliable assay technique was evolved and showed for the evaluation of zanubrutinib using reversed-phase high-performance liquid chromatography. Methods: In the proposed method, efficient chromatographic separation was achieved applying acetonitrile and 0.1% orthophosphoric acid (50:50 v/v) as a mobile phase with a flow of 1 ml/min and the wavelength was observed at 220 nm. Chromatography was administered isocratically at ambient temperature and run time was approximately 6 min and the retention time (Rt) was observed as 4.358 min. Results: The method was justified as per ICH guidelines. System suitability parameters were studied by injecting the quality six fold and results were well under acceptance criteria. Linearity study was administered between 10% and 150% levels, regression coefficient value was observed as 0.999. Limit of detection and limit of quantification were observed as 0.02 μg/ml and 0.2 μg/ml, respectively. Precision was found to be 0.74 for repeatability and 0.68 for intermediate precision. Recovery of the drug was found to be 98–102%, indicates that the recovery is in the acceptable limit. Validation results were found to be satisfactory and the method applicable for bulk and formulation analysis. Hence, it was evident that the proposed method was said to be suitable for regular analysis and quality control of pharmaceutical preparations. Conclusion: The validation results were in good agreement with the acceptable limit. Relative standard deviation values which are <2.0% indicating the accuracy and precision of this method. Assay of retail formulation was administered and found to be 100.24% was present using the above method. Stress conditions of degradation in acidic, alkaline, peroxide, and thermal were studied. This developed method showed reliable, precise, accurate results under optimized conditions.

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