Validated HPLC and Ultra-HPLC Methods for Determination of Dronedarone and Amiodarone Application for Counterfeit Drug Analysis

2015 ◽  
Vol 98 (6) ◽  
pp. 1496-1502 ◽  
Author(s):  
Ramzia I El-Bagary ◽  
Ehab F Elkady ◽  
Shereen Mowaka ◽  
Maria Attallah
Keyword(s):  
Flow Rate ◽  
Chromatographic Separation ◽  
Phosphate Buffer ◽  
Potassium Dihydrogen Phosphate ◽  
Pharmaceutical Preparations ◽  
Uv Detection ◽  
Dihydrogen Phosphate ◽  
Isocratic Elution ◽  
Potassium Dihydrogen

Abstract Two simple, accurate, and precise chromatographic methods have been developed and validated for the determination of dronedarone (DRO) HCl and amiodarone (AMI) HCl either alone or in binary mixtures due to the possibility of using AMI as a counterfeit of DRO because of its lower price. First, an RP-HPLC method is described for the simultaneous determination of DRO and AMI. Chromatographic separation was achieved on a BDS Hypersil C18 column (150 × 4.6 mm, 5 μm). Isocratic elution based on potassium dihydrogen phosphate buffer with 0.1% triethylamine pH 6–methanol (10 + 90, v/v) at a flow rate of 2 mL/min with UV detection at 254 nm was performed. The second method is RP ultra-HPLC in which the chromatographic separation was achieved on an AcclaimTM RSLC 120 C18 column (100 × 2.1 mm, 2.2 μm) using isocratic elution with potassium dihydrogen phosphate buffer with 0.1% triethylamine pH 6–methanol (5 + 95, v/v) at a flow rate of 1 mL/min with UV detection at 254 nm. Linearity, accuracy, and precision of the two methods were found to be acceptable over the concentration ranges of 5–80 μg/mL for both DRO and AMI. The results were statistically compared using one-way analysis of variance. The optimized methods were validated and proved to be specific, robust, precise, and accurate for the QC of the drugs in their pharmaceutical preparations.

A Validated HPLC Method for Simultaneous Determination of Perindopril Arginine, Amlodipine, and Indapamide: Application in Bulk and in Different Pharmaceutical Dosage Forms

2017 ◽  
Vol 100 (4) ◽  
pp. 992-999 ◽  
Author(s):  
Ramzia I El-Bagary ◽  
Ehab F Elkady ◽  
Shereen Mowaka ◽  
Maria A Attallah
Keyword(s):  
Potassium Dihydrogen Phosphate ◽  
Pharmaceutical Preparations ◽  
Dosage Forms ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Forms ◽  
Potassium Dihydrogen ◽  
Accuracy And Precision ◽  
Significant Difference

Abstract A simple, accurate, and precise LC method with a reversed stationary phase was developed and validated for the determination of perindopril (PER) arginine, amlodipine (AML), and indapamide (IND) alone and in binary mixtures (PER arginine is found in two dosage forms, i.e., with either AML or IND). Chromatographic separation was carried out on a BDS Hypersil® C18 column (100 × 3 mm, 5 μm). The mobile phase, consisting of 0.05 M potassium dihydrogen phosphate buffer (pH 2.6)–methanol (50 + 50, v/v), was pumped through the column whose temperature was maintained at 50°C at a flow rate of 0.6 mL/min using isocratic elution, and UV detection at 215 nm was performed. Acceptable values of linearity, accuracy, and precision of the method were found over the concentration ranges of 5–80 μg/mL PER, 2.5–80 μg/mL AML, and 0.5–20 μg/mL IND. The proposed chromatographic method was statistically compared to that of reference methods using one-way analysis of variance. The results showed that there was no significant difference between the methods. The developed method proved reliable for use in accurate QC of the drugs in their pharmaceutical preparations.

scholarly journals HPLC METHOD FOR DETERMINATION OF FLUOROMETHOLONE AND SODIUM CROMOGLYCATE IN BULK AND OPHTHALMIC SOLUTION Authors

2015 ◽  
Vol 7 ◽  
pp. 1
Author(s):  
Hani M. Hafez ◽  
Keyword(s):  
Sodium Cromoglycate ◽  
Flow Rate ◽  
Mobile Phase ◽  
Allergic Conjunctivitis ◽  
Potassium Dihydrogen Phosphate ◽  
Ophthalmic Solution ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen

Fluorometholone and Sodium Cromoglycate are used in the treatment of allergic conjunctivitis. A validated HPLC method was developed for the assay of them. The method was performed on BDS HYPERSIL C18 column (250x4.6 mm, 5μ) and the mobile phase consisted of potassium dihydrogen phosphate (pH 4.5, 0.025M) - Acetonitrile (40:60, V/V) which pumped at a flow rate 1.0 ml/min at ambient temperature. 20 µl of drugs sample solutions were monitored at two fixed wavelengths (lambda = 240.0 nm for Sodium Cromoglycate and 330.0 nm for Fluorometholone). The proposed method was validated in terms of linearity, accuracy, precision and limits of detection and quantitation according to ICH

DEVELOPMENT OF LIQUID CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS DETERMINATION OF BROMHEXINE HYDROCHLORIDE AND ENROFLOXACIN IN FORMULATIONS

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (02) ◽  
pp. 44-49
Author(s):  
P Choksi ◽  
◽  
F. Shaikh ◽  
D. A. Shah ◽  
K. Agarwal ◽  
...  
Keyword(s):  
Potassium Dihydrogen Phosphate ◽  
Fixed Dose ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Liquid Chromatographic Method ◽  
Dose Combination ◽  
Reproducible Method ◽  
Liquid Chromatographic ◽  
Isocratic Mode

A simple, specific, accurate, precise and reproducible method has been developed and validated for the estimation of bromhexine hydrochloride and enrofloxacin in fixed dose combination using RP-HPLC. The separation was achieved using stationary phase ODS Hypersil C18 column (250 mm× 4.6 mm i.d.) in isocratic mode, with mobile phase containing 0.05 M potassium dihydrogen phosphate buffer (pH 4 by o-phosphoric acid) : methanol: acetonitrile : triethylamine (40:20:40:01), at a flow rate of 1.0mL/min and eluents were monitored at 256 nm. The retention time of enrofloxacin and bromhexine HCl were found to be 3.00 min and 5.1 min respectively. The linearity for bromhexine HCl and enrofloxacin was in the range of 2-15 μg/mL and 20-150 μg/mL, respectively. The method was validated as per ICH guideline. The recoveries of bromhexine HCl and enrofloxacin were found in the range of 99.61-101.65% and 99.52-100.13 %, respectively. The method was successfully applied for the determination of both the drugs in combined dosage form.

Simultaneous Determination of 11 Aminoglycoside Residues in Honey, Milk, and Pork by Liquid Chromatography with Tandem Mass Spectrometry and Molecularly Imprinted Polymer Solid Phase Extraction

2017 ◽  
Vol 100 (6) ◽  
pp. 1869-1878 ◽  
Author(s):  
Bixia Yang ◽  
Lian Wang ◽  
Chunying Luo ◽  
Xixi Wang ◽  
Chengjun Sun
Keyword(s):  
Simultaneous Determination ◽  
Molecularly Imprinted Polymer ◽  
Solid Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Dihydrogen Phosphate ◽  
Imprinted Polymer ◽  
Ionization Source ◽  
Molecularly Imprinted ◽  
Potassium Dihydrogen

Abstract An analytical method was developed for the simultaneous determination of 11 aminoglycoside (AG) antibiotics, including amikacin, paromomycin, dihydrostreptomycin, gentamicin C1a, hygromycin, kanamycin, netilmicin, spectinomycin, sisomicin, streptomycin, and tobramycin in honey, milk, and pork samples by LC with tandem MS and molecularly imprinted polymer (MIP) SPE. The AG antibiotics in milk and homogenated meat samples were extracted with a solution composed of 10 mmol/L potassium dihydrogen phosphate, 0.4 mmol/L EDTA-Na2, and 2% trichloroacetic acid. For honey samples, the extractant was 50 mmol/L potassium dihydrogen phosphate. The extracts were cleaned up with MIP SPE cartridges. The separation was performed on a zwitter ionic-HILIC column (50 × 2.1 mm, 3.5 μm), with the mobile phase consisting of methanol, 0.3% formic acid, and 175 mmol/L ammonium formate at 0.50 mL/min in gradient elution. A triple-quadrupole mass spectrometer equipped with an electrospray ionization source, which was operated in positive mode, was used for detection. The quantification was based on matrix-matched calibration curves. The method was applied to real samples with three different matrixes. The LODs of the method were 2–30 μg/kg and the LOQs were 7–100 μg/kg; the average recovery ranged from 78.2 to 94.8%; intraday RSDs and interday RSDs were ≤15 and ≤18%, respectively; and the absolute values of matrix effect for all AGs were RSDs ≤23%.

scholarly journals Validation of Simultaneous Volumetric and HPLC Methods for the Determination of Pridinol Mesylate in Raw Material

2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Laura D. Simionato ◽  
Leonardo Ferello ◽  
Sebastián Stamer ◽  
Patricia D. Zubata ◽  
Adriana I. Segall
Keyword(s):  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Volumetric Method ◽  
Raw Material ◽  
Organic Layer ◽  
Dihydrogen Phosphate ◽  
Reverse Phase ◽  
Potassium Dihydrogen

Simple, sensitive, and economical simultaneous volumetric and HPLC methods for the determination of pridinol mesylate in raw material have been developed. The volumetric method is based on the reaction of pridinol with sodium lauryl sulphate in diluted sulphuric acid. Dimethyl yellow was used as indicator to detect the end point of the titration in aqueous/organic layer. The HPLC method for the determination of pridinol mesylate employs a reverse phase C18 column at ambient temperature with a mobile phase consisting of acetonitrile: 0.05 M potassium dihydrogen phosphate, pH adjusted to 5.0 (1 : 2, v/v). The flow rate was 0.8 mL/min. Quantitation was achieved with UV detection at 258 nm based on peak area. Both methods were found to be suitable for the quality control of pridinol mesylate in raw material.

scholarly journals The Determination of Metronidazole and Chlorhexidine Gluconate in Metronidazole and Chlorhexidine Lotion by HPLC

2022 ◽  
Vol 2152 (1) ◽  
pp. 012016
Author(s):  
Yun Yun ◽  
Mingshi Lin
Keyword(s):  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Chlorhexidine Gluconate ◽  
Dihydrogen Phosphate ◽  
Phosphate Solution ◽  
Phase Detection ◽  
Solution Ph ◽  
Tetrabutylammonium Hydroxide ◽  
Potassium Dihydrogen

Abstract Objective “To establish an HPLC method for the determination of metronidazole and chlorhexidine gluconate in metronidazole and chlorhexidine lotion. Method Using Agilent Eclipse-XDB-C18 chromatographic column, with 0.05 mol·L-1 potassium dihydrogen phosphate solution 1000 ml plus 13.2 ml 10% tetrabutylammonium hydroxide aqueous solution (pH adjusted to 3.5 by phosphoric acid)-acetonitrile (77:23) as Mobile phase, detection wavelength 230 nm. Results The two components could be separated well. The linear ranges of metronidazole and chlorhexidine acetate were 36.33~59.04 μg·ml-1 (r = 0.9994) and 35.45~220.11 μg·ml-1 (r = 1).); The average recoveries were 100.6% and 100.5 %, and the RSD were 0.42% and 0.58%. Conclusion: The method is simple and specific, and the result is more accurate and reliable. Which is suitable for simultaneous determination of two components in compound preparations.

scholarly journals RP-HPLC AND CHEMOMETRIC METHODS FOR THE DETERMINATION OF TWO ANTI-DIABETIC MIXTURES; METFORMIN HYDROCHLORIDE-CANAGLIFLOZIN AND METFORMIN HYDROCHLORIDE-GLICLAZIDE IN THEIR PHARMACEUTICAL FORMULATION

2019 ◽  
pp. 83-94
Author(s):  
MALAK Y. AL-BATHISH ◽  
AZZA A. GAZY ◽  
MARWA K. EL-JAMAL
Keyword(s):  
Binary Mixtures ◽  
Potassium Dihydrogen Phosphate ◽  
Pharmaceutical Preparations ◽  
Reversed Phase ◽  
Metformin Hydrochloride ◽  
Dihydrogen Phosphate ◽  
Control Analysis ◽  
Spectrophotometric Methods ◽  
Rp Hplc

Objective: To develop and validate novel more sensitive analytical methods for the concurrent quantification of metformin-canagliflozin and metformin-gliclazide in their bulk forms and in their pharmaceutical preparations. Methods: Two methods were developed based on several chemometric assisted spectrophotometric methods and a Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC). The first method applies different spectrophotometric chemometric assisted methods, including ratio difference, derivative ratio and extended ratio subtraction method, while the second method describes a RP-HPLC separation of metformin hydrochloride-canagliflozin and metformin hydrochloride-gliclazide binary mixtures using a C18 column with a mobile phase consisting of acetonitrile: potassium dihydrogen phosphate (adjusted to pH 3) with sodium lauryl sulphate as additive in the ratio of 30:70 (%v/v) in isocratic elution mode at 1 ml/min. Results: The proposed methods were able to quantify each of the studied drugs in their binary mixtures with high percentage recoveries in both methods. The spectrophotometric methods were able to quantify each of metformin, canagliflozin and gliclazide in the ranges of 2.0-20.0 μg/ml, 1.5-40.0 μg/ml and 2.0-30.0 μg/ml, respectively. The RP-HPLC method produced well-resolved peaks at a retention time of 3.92, 6.92 and 9.10 min in the concentration ranges of 50.0-300.0 μg/ml, 5.0-50.0 μg/ml and 10.0-100.0 μg/ml for metformin, canagliflozin and gliclazide, respectively. The proposed methods were optimized and validated in accordance to the International Conference of Harmonisation (ICH) guidelines in terms of linearity, LOD, LOQ, precision and accuracy. Conclusion: The developed methods were found to be sensitive and reproducible methods for the simultaneous determination of anti-diabetic binary mixtures; metformin hydrochloride-canagliflozin and metformin hydrochloride-gliclazide. And thus were successfully employed for the quality control analysis of the pharmaceutical formulations of the studied binary mixtures.

scholarly journals A Versatile Liquid Chromatographic Method for the Simultaneous Determination of Metformin, Sitagliptin, Simvastatin, and Ezetimibe in Different Dosage Forms

2018 ◽  
Vol 101 (2) ◽  
pp. 401-409 ◽  
Author(s):  
Asmaa A El-Zaher ◽  
Ehab F Elkady ◽  
Hanan M Elwy ◽  
Mahmoud Abo El Makarim Saleh
Keyword(s):  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Pharmaceutical Products ◽  
Metformin Hydrochloride ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Accuracy And Precision ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract A new LC method is introduced with the concept of its versatile application to widely used drugs from different pharmacological classes. Metformin hydrochloride (MTF), sitagliptin phosphate (SIT), simvastatin (SIM) and ezetimibe (EZB) were simultaneously determined with a simple reversed-phase LC method in which a SIT–SIM binary mixture, present in a dosage form brand, was considered central for its development. Chromatographic separation was achieved with a mobile phase of acetonitrile and 0.02 M potassium dihydrogen phosphate (pH 5.2) (77 + 23, v/v) flowing through a C18 column (BDS Hypersil, 250 × 4.6 mm, 5 µm) at 1.2 mL/min at ambient temperature. UV detection was programmed to be carried out at 210 nm for EZB, SIT, and MTF, whereas SIM was detected at 240 nm. The method was validated according to International Conference on Harmonization guidelines. Linearity, accuracy, and precision were satisfactory over concentration ranges 4–40 µg/mL for EZB and SIM, 0.5–50 µg/mL for SIT, and 5–500 µg/mL for MTF. Coefficients of determination were >0.99 for the four drugs. LOQs found were 0.01 µg/mL for EZB, 0.02 µg/mL for SIT, 0.2 µg/mL for MTF, and 0.02 µg/mL for SIM. The developed method is simple, rapid, accurate, precise, and suitable for the routine QC analysis of the cited drugs in pharmaceutical products by conventional HPLC systems.

Development and Validation of Rapid Ion-Pair RPLC Method for Simultaneous Determination of Certain B-Complex Vitamins Along with Vitamin C

2012 ◽  
Vol 95 (1) ◽  
pp. 74-83 ◽  
Author(s):  
Suyog S Patil ◽  
Ashwini K Srivastava
Keyword(s):  
Vitamin C ◽  
Simultaneous Determination ◽  
Potassium Dihydrogen Phosphate ◽  
Pharmaceutical Preparations ◽  
Clinical Analysis ◽  
Ion Pair ◽  
Dihydrogen Phosphate ◽  
Good Precision ◽  
B Complex Vitamins

Abstract A rapid, simple, and accurate ion-pair RPLC method has been developed for simultaneous analysis of vitamin C and major B-complex vitamins. An RP C18 column thermostated at 30°C was used with gradient elution of mobile phase comprising 10 mM potassium dihydrogen phosphate buffer (containing 3 mM sodium hexane-1-sulfonate, adjusted to pH 2.80 with o-phosphoric acid) and methanol at a flow rate of 1.0 mL/min to achieve the best possible separation and resolution of all vitamins in about 11.00 min. The detection was performed at 274 nm. The method has been implemented successfully for simultaneous determination of vitamins present in 12 multivitamin/multimineral pharmaceutical preparations, as well as in human urine. Typical validation characteristics were evaluated in accordance with International Conference on Harmonization guidelines. Good linearity over the investigated concentration levels was observed. Intraday repeatability was ≤2.0%, and interday variation was ≤2.6%, for all vitamins. The method can be used for assay of these vitamins over a wide concentration range with good precision and accuracy; hence, it would be appropriate for routine QC as well as in clinical analysis.

Sign in / Sign up

Export Citation Format

Share Document