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.

scholarly journals Development and Validation of a Novel Stability-Indicating RP-HPLC Method for Simultaneous Determination of Tezacaftor and Ivacaftor in Fixed Dose Combination

2020 ◽  
Vol 58 (4) ◽  
pp. 346-354
Author(s):  
Narendra Singh ◽  
Parveen Bansal ◽  
Mukesh Maithani ◽  
Yashpal Chauhan
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Reversed Phase ◽  
Fixed Dose ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Rp Hplc

Abstract A simple and precise novel stability-indicating method for the simultaneous estimation of tezacaftor and ivacaftor in combined tablet dosage form was developed and validated using reversed-phase high-performance liquid chromatography (RP-HPLC). The method is being reported for the first time and includes an estimation of degradation products produced post-stress conditions without any extraction or derivatization. The chromatographic separation of the drugs was achieved with a Symmetry Shield RP18 Column (100 Å, 5 μm, 4.6 mm × 250 mm) using a mixture of buffer, methanol and acetonitrile (42:27:31 v/v/v) as mobile phase. The buffer used in mobile phase contained 35 mM potassium dihydrogen phosphate, and its pH was adjusted to 7.0 ± 0.02 with 20% orthophosphoric acid. The instrument was set at flow rate of 1.2 mL min−1 at ambient temperature and the wavelength of UV-visible detector at 275 nm. The developed method could be suitable for the quantitative determination of these drugs in pharmaceutical preparations and also for quality control in bulk manufacturing. Stress testing was performed to prove the specificity. No interference was observed from its stress degradation products. The statistical analysis was done by using F-test and t-test at 95% confidence level.

scholarly journals Development and Validation of a Simple RP-HPLC Method for Simultaneous Estimation of Metformin Hydrochloride and Rosiglitazone in Pharmaceutical Dosage Forms

2013 ◽  
Vol 11 (2) ◽  
pp. 157-163
Author(s):  
Md Akteruzzaman ◽  
Asma Rahman ◽  
Md Zakir Sultan ◽  
Farhana Islam ◽  
Md Abdus Salam ◽  
...  
Keyword(s):  
Reversed Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Sodium Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

The objective of this study was to develop a simple, efficient, precise and accurate reversed phase HPLC (RP-HPLC) method for simultaneous determination of metformin in combination with rosiglitazone in newly formulated tablets. The combination of these drugs are commonly used and prescribed as anti-diabetic drugs in Bangladesh. The method has been developed by using the mobile phase comprising of sodium dihydrogen phosphate (NaH2PO4) buffer (pH 3.5) and acetonitrile (60:40, v/v) at a flow rate of 0.7 ml/min over C18 bonded silica column (ODS) (250 x 4.6 mm, 5 ?) at ambient temperature. The effluents were monitored at 230 nm and retention times were found to be 3.35 min and 11.95 min for metformin and rosiglitazone, respectively. Calibration curves were determined with a range from 0.03125 to 0.50 ?mole/ml of standards and the regression coefficients (r2) were found as 0.999 for metformin and 1.0 for rosiglitazone. The assay was validated for the accuracy, precision etc. according to ICH, USP and FDA guidelines. The proposed method can be useful in routine analysis for quantitative determination of metformin hydrochloride and rosiglitazone in pharmaceutical dosage forms. DOI: http://dx.doi.org/10.3329/dujps.v11i2.14574 Dhaka Univ. J. Pharm. Sci. 11(2): 157-163, 2012 (December)

scholarly journals A Rapid Stability-Indicating RP-HPLC Method for the Determination of Betaxolol Hydrochloride in Pharmaceutical Tablets

2013 ◽  
Vol 8 ◽  
pp. ACI.S11256 ◽  
Author(s):  
Sylvain Auvity ◽  
Fouad Chiadmi ◽  
Salvatore Cisternino ◽  
Jean-Eudes Fontan ◽  
Joël Schlatter
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Rp Hplc

A stability-indicating reversed-phase high performance liquid chromatography (RP-HPLC) method was developed for the determination of betaxolol hydrochloride, a drug used in the treatment of hypertension and glaucoma. The desired chromatographic separation was achieved on a Nucleosil C18, 4 μm (150 × 4.6 mm) column, using isocratic elution at a 220 nm detector wavelength. The optimized mobile phase consisted of a 0.02 M potassium dihydrogen phosphate: methanol (40:60, v/v, pH 3.0 adjusted with o-phosphoric acid) as solvent. The flow rate was 1.6 mL/min and the retention time of betaxolol hydrochloride was 1.72 min. The linearity for betaxolol hydrochloride was in the range of 25 to 200 μg/mL. Recovery for betaxolol hydrochloride was calculated as 100.01%-101.35%. The stability-indicating capability was established by forced degradation experiments and the separation of unknown degradation products. The developed RP-HPLC method was validated according to the International Conference on Harmonization (ICH) guidelines. This validated method was applied for the estimation of betaxolol hydrochloride in commercially available tablets.

STABILITY INDICATING UPLC METHOD FOR ESTIMATION OF METFORMIN HYDROCHLORIDE AND NATEGLINIDE SIMULTANEOUSLY IN THE PRESENCE OF STRESS DEGRADATION PRODUCTS

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (05) ◽  
pp. 56-64
Author(s):  
Rani A Prameela ◽  
S. Madhavi ◽  
Rao B. Tirumaleswara ◽  
Sudheer Reddy CH.
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Metformin Hydrochloride ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Column Temperature

A novel Ultra Performance Liquid Chromatography (UPLC) method was developed and validated for the simultaneous determination of antidiabetic drugs metformin hydrochloride and nateglinide. The method was developed using a Waters ACQUITY UPLC SB C18 (100 × 2.1 mm, 1.8 μm) column. The mobile phase consisting of 0.01 % potassium dihydrogen phosphate buffer (pH 5.8): acetonitrile (50: 50 V/V) was used throughout the analysis. The flow rate was 0.3 mL/min, the injection volume was 1.0 μL, column temperature was 30 0C, run time 3 min and detection was carried at 238 nm using a TUV detector. The retention times of metformin hydrochloride and nateglinide were found to be 1.28 1.71 min, respectively. Metformin hydrochloride and nateglinide were found to be linear over the concentration range of 125-750 and 15-90 μg/mL. The limit of detection and the limit of quantification for metformin hydrochloride were found to be 0.22 and 0.68 μg/mL, respectively, and, for nateglinide, 0.02 and 0.6 μg/mL, respectively. Developed method was validated as per ICH guidelines. The specificity of the method was confirmed by forced degradation study. The suggested method is suitable for determination of metformin hydrochloride and nateglinide in bulk and pharmaceutical dosage forms.

scholarly journals Development and validation of a reversed-phase HPLC method for determination of assay content of Teriflunomide by the aid of BOMD simulations

2021 ◽  
pp. 281-294 ◽  
Author(s):  
Abolghasem Beheshti ◽  
Zahra Kamalzadeha ◽  
Monireh Haj-Maleka ◽  
Meghdad Payaba ◽  
Mohammad Amin Rezvanfar ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Td Dft ◽  
High Level ◽  
Development And Validation

Due to the new hopes for treatment of multiple sclerosis (MS) diseases by Teriflunomide (TFN), in this project, a cheap, robust, and fully validated method has been developed both for determination of assay content in API (active pharmaceutical ingredient), and for related impurities analysis (RIA). To operate the method, a common C18, end-capped (250 × 4.6) mm, 5µm liquid chromatography column, was applied. The mobile phase A was prepared by dissolving 2.74 g (20mM) of PDP (potassium dihydrogen phosphate) and 3.72 g (50mM) of PC (potassium chloride) in water (1000 mL). Then, pH was adjusted to 3.0 by adding OPA (ortho-phosphoric acid) 85%; while, the mobile phase B was acetonitrile (ACN) (100%). In order to confirm the experimental data about the λmax of TFN, we have used the Born-Oppenheimer molecular dynamics (BOMD) simulations, quantum mechanics (QM), and TD-DFT calculations. According to the results, the method showed a high level of suitability, specificity, linearity, accuracy, precision, repeatability, robustness, and reliable detection limit.

Determination of Dephosphate Bromofenofos in Milk by Liquid Chromatography with Electrochemical Detection

1994 ◽  
Vol 77 (4) ◽  
pp. 904-908 ◽  
Author(s):  
Kazue Takeba ◽  
Takeshi Itoh ◽  
Masao Matsumoto ◽  
Hiroyuki Nakazawa
Keyword(s):  
Liquid Chromatography ◽  
Electrochemical Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Dihydrogen Phosphate ◽  
Specific Method ◽  
Coefficients Of Variation ◽  
The Matrix

Abstract A sensitive, specific method for the determination of dephosphate bromofenofos (DBFF) in milk by liquid chromatography (LC) with electrochemical detection is described. DBFF, the only metabolite of bromofenofos (BFF, a fasciolicide), was extracted from milk by liquid–liquid partition with acetone, acetonitrile, and dichloromethane and purified by using a C18 cartridge. The compound was separated from the matrix peaks by reversed-phase LC and detected by dual-electrode coulometric detection on a Kaseisorb LC ODS-300-5 (250 × 4.6 mm id, 5 μm) column. The mobile phase was acetonitrile–0.05M potassium dihydrogen phosphate (55 + 45, v/v) at pH 3.0. The flow rate was 1 mL/min at 40°C. The applied potentials of detectors 1 and 2 were maintained at 0.30 and 0.45 V, respectively. Average recoveries (n = 5) of DBFF from milk spiked at 1 and 10 ng/mL were 73.1 and 82.7%, respectively; and coefficients of variation were 8.4 and 2.8%, respectively. The detection limit of DBFF in milk was 0.2 ng/mL. Fifty-nine raw and 181 commercial milks were analyzed. DBFF was detected in 4 raw milks (0.2–1.5 ng/mL; average, 0.6 ng/mL) and in 3 normal liquid commercial milks (0.3–0.7 ng/mL; average, 0.5 ng/mL). The identity of DBFF from milk was confirmed by gas chromatography/mass spectrometry.

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 Determination of Five Fasciolicides in Milk by Liquid Chromatography with Electrochemical Detection

1996 ◽  
Vol 79 (4) ◽  
pp. 848-852 ◽  
Author(s):  
Kazue Takeba ◽  
Takeshi Itoh ◽  
Masao Matsumoto ◽  
Hlroyuki Nakazawa ◽  
Shinzo Tanabe
Keyword(s):  
Liquid Chromatography ◽  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Dihydrogen Phosphate ◽  
Specific Method ◽  
Hydrogen Carbonate ◽  
The Matrix ◽  
Phase Liquid ◽  
Liver Flukes

Abstract A sensitive and specific method is described for determination of 5 fasciolicides in milk. The drugs are used to control liver flukes in cattle. The milk sample was homogenized with acetone and acetonitrile, sonicated, and centrifuged. The supernatant was extracted with dichloromethane. The extract was evaporated to dryness, dissolved in 1 % sodium hydrogen carbonate, and purified on a C18 cartridge. The 5 drugs were separated from the matrix by reversed-phase liquid chromatography (LC) and determined by dual-electrode coulometric detection on a Kaseisorb LC ODS-300-5 column. The mobile phase was acetonitrile-0.05M potassium dihydrogen phosphate (55 + 45) at pH 3.0. The flow rate was 1 mL/min at 40°C. The applied potentials of detectors 1 and 2 were set at 0.20 and 0.55 V, respectively. The average recovery of the drugs added to milk at 0.01 and 0.1 µ g/mL was 89.6%, and the coefficient of variation was 4.7%. The detection limits of the drugs in milk were 4-20 ng/mL. The method is used to monitor commercial milk samples and to determine the residual levels of these drugs in milk from cows treated with a fasciolicide.

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

2012 ◽  
Vol 2012 ◽  
pp. 1-9 ◽  
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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