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.

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.

scholarly journals Simultaneous HPLC Determination of Chlordiazepoxide and Mebeverine HCl in the Presence of Their Degradation Products and Impurities

2015 ◽  
Vol 2015 ◽  
pp. 1-9
Author(s):  
Rania N. El-Shaheny ◽  
Fathalla F. Belal
Keyword(s):  
Simultaneous Determination ◽  
Degradation Product ◽  
Mobile Phase ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Ir Studies ◽  
Validation Procedure

A simple, rapid, and sensitive RP-HPLC method was developed and validated for the simultaneous determination of chlordiazepoxide (CDO) and mebeverine HCl (MBV) in the presence of CDO impurity (2-amino-5-chlorobenzophenone, ACB) and MBV degradation product (veratric acid, VER). Separation was achieved within 9 min on a BDS Hypersil phenyl column (4.5 mm × 250 mm, 5 µm particle size) using a mobile phase consisting of acetonitrile: 0.1 M potassium dihydrogen phosphate: triethylamine (35 : 65 : 0.2, v/v/v) in an isocratic mode at a flow rate of 1 mL/min. The pH of the mobile phase was adjusted to 4.5 with orthophosphoric acid and UV detection was set at 260 nm. A complete validation procedure was conducted. The proposed method exhibited excellent linearity over the concentration ranges of 1.0–100.0, 10.0–200.0, 2.0–40.0, and 2.0–40.0 µg/mL for CDO, MBV, VER, and ACB, respectively. The proposed method was applied for the simultaneous determination of CDO and MBV in their coformulated tablets with mean percentage recoveries of 99.75 ± 0.62 and 98.61 ± 0.38, respectively. The results of the proposed method were favorably compared with those of a comparison HPLC method using Studentt-test and the variance ratioF-test. The chemical structure of MBV degradation product was ascertained by mass spectrometry and IR studies.

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 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.

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 Simultaneous Estimation of Satranidazole and Ofloxacin in Tablet Dosage Form by High Performance Liquid Chromatography

2010 ◽  
Vol 7 (1) ◽  
pp. 198-202 ◽  
Author(s):  
R. Shinde Sachin ◽  
I. Bhoir Suvarna ◽  
S. Pawar Namdev ◽  
B.Yadav Suman ◽  
M. Bhagwat Ashok
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Standard Addition ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Tablet Dosage

A Simple, fast and precise reversed phase high performance liquid chromatographic method is developed for the simultaneous determination of satranidazole and ofloxacin. Chromatographic separation of these drugs were performed on Kromasil C18column (250 x 4.6 mm, 5 µ) as stationary phase with a mobile phase comprising of 20 mM potassium dihydrogen phosphate: acetonitrile in the ratio of 60:40 (v/v) containing 0.1% glacial acetic acid at a flow rate of 1 mL/min and UV detection at 318 nm. The linearity of satranidazole and ofloxacin were in the range of 1.5 to 3.6 µg/mL and 1.0 to 2.4 µg/mL respectively. The recovery was calculated by standard addition method. The average recovery was found to be 100.63% and 100.02% for satranidazole and ofloxacin respectively. The proposed method was found to be accurate, precise and rapid for simultaneous determination of satranidazole and ofloxacin

Simultaneous Determination of Metformin, Glipizide, Repaglinide, and Glimepiride or Metformin and Pioglitazone by a Validated LC Method: Application in the Presence of Metformin Impurity (1-Cyanoguanidine)

2016 ◽  
Vol 99 (4) ◽  
pp. 957-963 ◽  
Author(s):  
Asmaa A El-Zaher ◽  
Ehab F Elkady ◽  
Hanan M Elwy ◽  
Mahmoud A Saleh
Keyword(s):  
Simultaneous Determination ◽  
Potassium Dihydrogen Phosphate ◽  
Correlation Coefficients ◽  
Pharmaceutical Formulations ◽  
Pharmaceutical Products ◽  
Metformin Hydrochloride ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Accuracy And Precision

Abstract A rapid, simple, and precise RPLC method was developed for the simultaneous determination of the widely used oral antidiabetic, metformin hydrochloride (MTF), with some commonly coadministered oral antidiabetics from different pharmacological classes—glipizide (GPZ), pioglitazone hydrochloride (PGZ), glimepiride (GLM), and repaglinide (RPG)—in bulk, laboratory-prepared mixtures and pharmaceutical formulations in the presence of metformin-reported impurity [1-cyanoguanidine (CNG)]. Chromatographic separation was achieved using isocratic elution mode with a mobile phase of acetonitrile: 0.02 M potassium dihydrogen phosphate (pH 3.17; 50–50, v/v) flowing through a CN Phenomenex column (Phenosphere Next, 250 × 4.6 mm, 5 μm) at a rate of 1.5 mL/min at ambient temperature. UV detection was carried out at 220 nm. The method was validated according to International Conference on Harmonization guidelines. Linearity, accuracy, and precision were satisfactory for concentration ranges: 0.175–350 μg/mL for MTF, 0.0525–105 μg/mL for GPZ, 0.125–250 μg/mL for PGZ, and 0.05–100 μg/mL for GLM and RPG. Correlation coefficients were >0.99 for all analytes. LOQs were 0.009 μg/mL for MTF, 0.009 μg/mL for GPZ, 0.04 μg/mL for GLM, 0.124 μg/mL for PGZ, and 0.044 μg/mL for RPG. The developed method is specific, accurate, and suitable for the QC and routine analysis of the cited drugs in their pharmaceutical products.

Development of LC Method for the Simultaneous Determination of Antidepressant Drug Combination Melitracen Hydrochloride and Flupentixol Dihydrochloride in their Combined Dosage Form

2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
Usmangani K. Chhalotiya ◽  
Kashyap K. Bhatt ◽  
Dimal A. Shah ◽  
Gautam R. Chauhan ◽  
Sunil L. Baldania
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Dosage Form ◽  
Antidepressant Drug ◽  
Potassium Dihydrogen Phosphate ◽  
Chemical Oxidation ◽  
Reversed Phase ◽  
Dihydrogen Phosphate ◽  
Tablet Dosage

A simple, specific and stability-indicating reversed-phase high-performance liquid chromatographic method was developed for the simultaneous determination of melitracen hydrochloride and flupentixol dihydrochloride in tablet dosage form. A Brownlee C-18, 5 μm column having 250×4.6 mm i.d. in isocratic mode, with mobile phase containing 0.025 M potassium dihydrogen phosphate: methanol (10 : 90, v/v; pH 7.3) was used. The flow rate was 1.0 mL/min, and effluents were monitored at 230 nm. The retention times of melitracen hydrochloride and flupentixol dihydrochloride were 7.75 min and 5.50 min, respectively. The linearity for melitracen hydrochloride and flupentixol dihydrochloride were in the range of 0.5–60 μg/mL. The recoveries obtained for melitracen hydrochloride and flupenthixol dihydrochloride was 99.81–100.77% and 99.42–100.12%, respectively. Both the drugs were subjected to acid and alkali hydrolysis, chemical oxidation, and dry heat degradation and photodegradation. The proposed method was validated and successfully applied to the estimation of melitracen hydrochloride and flupentixol dihydrochloride in combined tablet dosage form.

scholarly journals A quantitative HPLC method for simultaneous determination of prodrug of voriconazole and voriconazole in beagle plasma, and its application to a toxicokinetic study

2021 ◽  
Author(s):  
Yufa Wen ◽  
Shuang Chen ◽  
Yanjuan Yuan ◽  
Qing Shao ◽  
Xuejun He ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Internal Standard ◽  
Storage Conditions ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Different Temperatures ◽  
Reproducible Method

AbstractA simple, rapid, efficient and reproducible method based on High Performance Liquid Chromatography (HPLC) for simultaneous determination of prodrug of voriconazole (POV) and voriconazole in beagle plasma has been established and validated. Omeprazole was utilized as the sole internal standard. Analytes and internal standards were extracted through protein precipitation and separated on a Venusil XBP C18 chromatography column (4.6 × 250 mm, 5 µm). The mobile phase was methanol and 20 mmol/L potassium dihydrogen phosphate. Chromatographic separation was achieved by using an isocratic elution procedure that used 65% methanol and a flow rate of 1 mL/min. The ultraviolet (UV) detection wavelength was 256 nm and the total running time was 15 min. This method showed good linear ranges of 100–75,000 ng/mL for voriconazole prodrug and 200–100,000 ng/mL for voriconazole respectively. The precision and accuracy were acceptable. Analytes in plasma samples are stable under different temperatures and storage conditions. The developed HPLC method has been successfully applied to the studies of toxicokinetics of POV after intravenous drip in beagle and provided important information for the further development and application.

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