scholarly journals Simultaneous quantification of empagliflozin, linagliptin and metformin hydrochloride in bulk and synthetic mixture by RP–LC method

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Ishita M. Patel ◽  
Usmangani K. Chhalotiya ◽  
Harsha D. Jani ◽  
Devansh Kansara ◽  
Hetaben M. Kachhiya ◽  
...  
Keyword(s):  
High Performance ◽  
Hplc Method ◽  
Synthetic Mixture ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Extensive Literature ◽  
Isocratic Elution ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Metformin Hcl

Abstract Background Extensive literature review revealed that no RP–LC method has been developed for simultaneous estimation of EMPA, LINA and MET in combined dosage form. This is a newer combination approved by USFDA on 4th June 2019 and it is launch in the United State Market on 27th January 2020. Result A simple, sensitive, specific, precise and accurate reverse phase—high performance liquid chromatography (RP- HPLC) method has been developed for simultaneous estimation of Empagliflozin, Linagliptin and Metformin HCl in bulk and synthetic mixture. Phenomenex C18 column (250 mm × 4.6 mm, 5 µm) was used as stationary phase for chromatographic separation through isocratic elution using Acetonitrile: Methanol: Water in a ratio (27: 20: 53, v/v/v) pH 4 adjusted with 1% Ortho-phosphoric acid as mobile phase at flow rate 1 ml/min. PDA detector was used for simultaneous analysis of all three drugs at common wavelength 223 nm and the each injection volume was 20 µl. The linearity range for Empagliflozin, Linagliptin and Metformin HCl was found to be 0.5–5 µg/ml, 0.25–2.5 µg/ml, and 50–500 µg/ml, respectively. The retention time for Empagliflozin, Linagliptin and Metformin HCl was found to be 14.5 min, 3.4 min and 2.01 min, respectively. The percentage (%) recovery was found to be 99.98–100.81% for Empagliflozin, 99.33–100.57% for Linagliptin and 100.65–101.35% for Metformin HCl respectively. Conclusion As per the international Conference on Harmonisation (ICH) Q2 (R1) guideline, proposed RP–LC method validation has been carried out. The proposed RP–LC method was repeatable and selective as per statistical analysis and it can be use for simultaneous estimation of Empagliflozin, Linagliptin and Metformin HCl in bulk and synthetic mixture. The proposed method might be applied for simultaneous estimation of all three drugs in pharmaceutical formulation.

scholarly journals A VALIDATED RP-HPLC METHOD FOR IMPURITY PROFILING OF SODIUM NITROPRUSSIDE IN INJECTION DOSAGE FORM

2021 ◽  
pp. 160-169
Author(s):  
MURALI KRISHNAM RAJU P. ◽  
VENKATA NARAYANA B. ◽  
SHYAMALA P. ◽  
SRINIVASU KONDRA ◽  
HSN RAJU DANTULURI
Keyword(s):  
Sodium Nitroprusside ◽  
High Performance ◽  
Research Work ◽  
Hplc Method ◽  
Isocratic Elution ◽  
Reverse Phase ◽  
Impurity Profiling ◽  
Rp Hplc ◽  
Acceptance Range ◽  
Nitrite Nitrate

Objective: The main objective of this research work is to develop and validate a single reverse-phase high-performance liquid chromatography (RP-HPLC) method. This method should becapable of quantifying all the known, as well as other possible degradation impurities of sodium nitroprusside (SNP) in its injection formulation. Methods: Of allmethod development trails, we have observed better separations between known and degradation impuritiesin Inert sustain C18, (250 x 4.6) mm, 5 µm column at 30 °C temperature. Isocratic elution was carried out by using pH 8.6 phosphate buffer and acetonitrile in the ratio of 65:35 %v/v with a flow rate of 0.8 ml/min. The detection was carried out at 220 nm, with an injection volume of 10 µl. Results: In the proposed method, SNP was eluted at 22.5 min. Nitrite, nitrate, and ferrocyanide were linear from 0.25 to 37 μg/ml, ferricyanide was linear from 1.0 to 37 μg/ml, and SNP was linear from 0.75 to 37 μg/ml. The % RSD for six spiked samples (precision)was found to be less than 0.5 %. Accuracy was performed for known impurities from LOQ to 150 % for a 0.5 % specification level. The resultswere found to be in the acceptance range of 90-110 %. The LOQ concentration of nitrite, nitrate, and ferrocyanide was 0.25 μg/ml each,LOQ offerricyanide and SNP was found to be 1.0 μg/ml and 0.75 μg/ml, respectively. The SNP injection samples were exposed to different degradation conditions, and the results were found specific in the proposed methodology. Conclusion: The proposed RP-HPLC method is specific, precise, accurate, linear, stable, and robust for quantification of known and other possible degradation impurities in SNP injection formulation.

scholarly journals SIMULTANEOUS ESTIMATION AND FORCED DEGRADATION STUDIES OF AMILORIDE HYDROCHLORIDE AND FUROSEMIDE IN A PHARMACEUTICAL DOSAGE FORM USING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD

2018 ◽  
Vol 11 (7) ◽  
pp. 215 ◽  
Author(s):  
Javed S Shaik ◽  
Nutan N Rao
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Uv Detector ◽  
Reverse Phase ◽  
Rp Hplc ◽  
The Stability ◽  
Amiloride Hydrochloride

Objective: The present study describes the stability indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous estimation of amiloride hydrochloride and furosemide in pharmaceutical dosage forms.Methods: The proposed RP-HPLC method was developed using Shimadzu LC-2030 HPLC system equipped with UV detector, and chromatographic separation was carried on Shim-pack C18 (250 mm×4.6 mm, 5 μ) column at a flow rate of 1 ml/min and the runtime was 4min. The mobile phase consisted of water and acetonitrile in the ratio of 35:65, and elements were scanned using a UV detector at 281 nm.Results: The retention time of amiloride hydrochloride and furosemide was found to be 1.92 min and 3.14min, respectively. Linearity was found to be 12–28 ppm for amiloride hydrochloride and 96–224 ppm for furosemide, respectively. Limit of detection and limit of quantification for amiloride hydrochloride were 0.381 ppm and 1.156 ppm and for furosemide were 2.00 ppm and 6.068 ppm, respectively.Conclusion: The stability indicating method was developed by subjecting the drugs to stress conditions such as acid and base hydrolysis, oxidation, humidity, photolytic, and thermal degradation, and the degraded products formed were resolved successfully from the samples.

scholarly journals Novel HPLC Analysis of Hydrocortisone in Conventional and Controlled-Release Pharmaceutical Preparations

2017 ◽  
Vol 2017 ◽  
pp. 1-8 ◽  
Author(s):  
Ofosua Adi-Dako ◽  
Samuel Oppong Bekoe ◽  
Kwabena Ofori-Kwakye ◽  
Enoch Appiah ◽  
Paul Peprah
Keyword(s):  
Controlled Release ◽  
High Performance ◽  
Pharmaceutical Preparations ◽  
Hplc Method ◽  
Isocratic Elution ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Significant Difference ◽  
Interday Precision ◽  
Concentration Levels

An isocratic sensitive and precise reverse phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the determination and quantification of hydrocortisone in controlled-release and conventional (tablets and injections) pharmaceutical preparations. Chromatographic separation was achieved on an ODS (C18), 5 μm, 4.6 × 150 mm, with an isocratic elution using a freshly prepared mobile phase of composition methanol : water : acetic acid (60 : 30 : 10, v/v/v) at a flow rate of 1.0 ml/min. The detection of the drug was successfully achieved at a wavelength of 254 nm. The retention time obtained for the drug was 2.26 min. The proposed method produced linear detectable responses in the concentration range of 0.02 to 0.4 mg/ml of hydrocortisone. High recoveries of 98–101% were attained at concentration levels of 80%, 100%, and 120%. The intraday and interday precision (RSD) were 0.19–0.55% and 0.33–0.71%, respectively. A comparison of hydrocortisone analyses data from the developed method and the official USP method showed no significant difference (p>0.05) at a 95% confidence interval. The method was successfully applied to the determination and quantification of hydrocortisone in six controlled-release and fifteen conventional release pharmaceutical preparations.

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION OF LAMIVUDINE AND ZIDOVUDINE IN TABLET BY REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2020 ◽  
pp. 73-77
Author(s):  
BHOOMI D PATEL ◽  
MEHTA BHAVYA ◽  
ANKIT B CHAUDHARY
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Rp Hplc

Objective: The objective of the study was to develop and validate reverse-phase high-performance liquid chromatography (RP-HPLC) method and apply method to tablet dosage form. Methods: A simple, rapid, economical, precise, and accurate RP-HPLC method for simultaneous estimation of lamivudine and zidovudine in their combined dosage form has been developed. Results: A RP-HPLC method was developed for the simultaneous estimation of lamivudine and zidovudine. In their combined dosage form has been developed. The separation was achieved by LC-C18 column (150 mm ×4.6 mm, 5 μm) and water: methanol (65:35v/v) as mobile phase, at a flow rate of 0.8 ml/min. Detection was carried out at 272 nm. Retention time of lamivudine and zidovudine was found to be 3.007 min and 4.647, respectively. The method has been validated for linearity, accuracy, and precision. The assay method was found to be linear from 50% to 150% for lamivudine and zidovudine. Conclusion: Developed method was found to be accurate, precise, and rapid for simultaneous estimation of lamivudine and zidovudine in their combined dosage form.

scholarly journals DEVELOPMENT AND VALIDATION OF REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR SIMULTANEOUS ESTIMATION OF OLANZAPINE AND ARIPIPRAZOLE IN SYNTHETIC MIXTURES

2020 ◽  
pp. 162-168
Author(s):  
MEGHA PATEL ◽  
PARESH PATEL ◽  
DHARA PATEL
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Reverse Phase ◽  
Chromatography Method ◽  
Rp Hplc ◽  
Liquid Chromatography Method

Objective: A simple, rapid, accurate, precise, specific, and sensitive reverse-phase high-performance liquid chromatography (RP-HPLC) method has been developed and validated for simultaneous estimation of olanzapine (OLZ) and aripiprazole (APR) in synthetic mixtures. Methods: The stationary phase used for chromatographic separation was Phenomenex C18 column (250 mm × 4.6 mm i.d, particle size 5 μm) and mobile phase used for separation was methanol: Phosphate buffer (pH 3) taken in ratio of 75:25 %v/v. The flow rate was used 1.0 ml/min at room temperature and drugs detected at 240 nm with injection volume 20 μL. Results: The retention time for OLZ and APR was found to be 4.231 and 6.523 min, respectively. The linearity was performed using a concentration range of 0.5–3.0 for both drugs. The correlation coefficient was found to be 0.999 for OLZ and APR. The % purity of both the drug was found to be 98–102%. The proposed RP-HPLC method has been validated, according to International council on harmonization Q2 (B) guidelines. Conclusion: There was no interference of any diluents and excipients in the determination of drugs from synthetic mixture. Hence, the developed method can be used for routine quality control analysis.

scholarly journals A VALIDATED ANALYTICAL METHOD FOR THE SIMULTANEOUS ESTIMATION OF CYTARABINE AND DAUNORUBICIN IN BULK AND INFUSION FORMULATION BY REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

2019 ◽  
pp. 128-131 ◽  
Author(s):  
PRASANTHI CHENGALVA ◽  
LATHA LAVANYA PEDDAVENGARI ◽  
MADHAVI KUCHANA
Keyword(s):  
High Performance ◽  
Quantitative Estimation ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Column Temperature ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Relative Standard

Objective: The novel liposomal infusion formulation of cytarabine and daunorubicin liposomal infusion is considered as new hope in acute myeloid leukemia treatment. The objective of the present study is to develop and validate a simple, rapid, accurate, precise and sensitive reverse-phase high-performance liquid chromatographic (RP-HPLC) method for the simultaneous estimation of cytarabine and daunorubicin in bulk and infusion formulation. Methods: The chromatographic separation of the drugs was achieved on Denali C18 (250 mm×4.6 mm, 5 μm) in isocratic mode with mobile phase consisting of water (pH was adjusted to 3):acetonitrile in the ratio of 55:45 with a flow rate of 1 ml/min at a detection wavelength of 240 nm using photodiode array (PDA) detector. The column temperature was set at 30°C with 10 μl injection volume. The proposed method was validated as per the International council for Harmonisation (ICH) guidelines. Results: The retention times for cytarabine and daunorubicin were found to be 2.323±0.12 min and 3.140±0.16 min, respectively. Linearity (r2=0.999) was observed over a concentration range of 16.2–97.5 μg/ml for cytarabine and 7.2–43.5 μg/ml for daunorubicin. The percentage relative standard deviation (RSD) for precision studies was found to be 0.2 for both the drugs. Conclusion: A simple, rapid, economic, accurate, and precise RP-HPLC method was developed for simultaneous quantitative estimation of cytarabine and daunorubicin, and the method was validated as per the ICH guidelines. Hence, the method can be employed for the routine analysis of cytarabine and daunorubicin in bulk and infusion formulation.

scholarly journals Simultaneous estimation of pioglitazone, glimepiride & metformin hydrochloride in bulk & tablet dosage form by UV, RP-HPLC method

2021 ◽  
Vol 8 (3) ◽  
pp. 91-99
Author(s):  
Shoheb S Shaikh ◽  
Nachiket S Dighe
Keyword(s):  
High Performance ◽  
Spectroscopic Method ◽  
Hplc Method ◽  
Isosbestic Point ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Drug Substances ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Tablet Dosage

A stability-indicating UV spectroscopic and high-performance liquid chromatography (RP-HPLC) method is developed for the quantification ofPioglitazone, Glimepiride & Metformin Hydrochloride drug substances. UV spectroscopic method was developed and validated, the wavelength selected for simultaneous estimation were 226nm for pioglitazone, 229nm for glimepiride and 232nm for metformin hydrochloride. The isosbestic point found for the analysis was 229nm. Selected mobile phase was a combination of methanol and water with a ratio of 70% Methanol and 30 % HPLC water with the flow rate of 0.85ml/min. The analyte was analysed on the C18 HPLC column having the pore size of 5 microns at room temperature. The method is validated according to ICH guidelines, the retention time of about 4.0min for metformin, 5.5min for Pioglitazone and 6.8min for Glimepiride was observed. The linearity range with regression co-efficient for Pioglitazone, Glimepiride & Metformin Hydrochloride is 3-15 μg/mL,0.4-1.2 μg/mL and 100-500 μg/mL and 0.9998, 0.9991, 0.9991 respectively.

scholarly journals Development and validation of stability-indicating RP-HPLC method for the simultaneous determination of ertugliflozin pidolate and metformin hydrochloride in bulk and tablets

2020 ◽  
Vol 6 (1) ◽  
Author(s):  
K. Sravana Kumari ◽  
Sailaja Bandhakavi
Keyword(s):  
Hplc Method ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Standard Solution ◽  
Development And Validation ◽  
Metformin Hcl

Abstract Background In the present study, an improved simple, specific, rapid, sensitive, precise, accurate and stability-indicating RP-HPLC method for the simultaneous estimation of ertugliflozin pidolate and metformin hydrochloride in bulk and tablets was developed and validated. The separation of ertugliflozin pidolate and metformin HCl was achieved isocratically on Kromasil C18 column (150 mm × 4.6 mm, 5 μm) using 0.1% ortho-phosphoric acid buffer (pH 2.7):acetonitrile (65:35% v/v) as mobile phase, pumped at a flow rate of 1 ml/min and column temperature of 30 ± 2 °C. HPLC grade water:ACN (1:1) was used as diluent. About 10 μl of standard solution of the drugs was injected, and the eluted analytes were detected at 224 nm. Results Metformin HCl was eluted at 2.170 min and ertugliflozin pidolate at 2.929 min with a run time of 5.0 min. Linearity of the developed method was observed in the concentration range of 0.9375–5.625 μg/ml for ertugliflozin pidolate and 62.5–375 μg/ml for metformin HCl with a correlation coefficient of 0.999 for both the drugs. LOD for ertugliflozin pidolate and metformin HCl were 0.025 μg/ml and 0.87 μg/ml respectively. LOQ for ertugliflozin pidolate and metformin HCl were 0.076 μg/ml and 2.63 μg/ml. Conclusion The developed RP-HPLC method for the simultaneous estimation of ertugliflozin pidolate and metformin HCl in bulk and tablets was simple, rapid, sensitive, accurate, precise, linear, and stability indicating. Hence, the developed method could be used for the routine quality control of the drugs in bulk and tablets.

scholarly journals A A RAPID AND SENSITIVE RP-HPLC METHOD FOR THE QUANTITATIVE ANALYSIS OF EMPAGLIFLOZIN IN BULK AND PHARMACEUTICAL DOSAGE FORM

2019 ◽  
pp. 60-65
Author(s):  
MADHURIMA BASAK ◽  
Santhosh Reddy Gouru ◽  
Animesh Bera ◽  
Krishna veni Nagappan
Keyword(s):  
Quantitative Analysis ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Bulk Drug

Objective: The present study aims at developing an accurate precise, rapid and sensitive Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) method for assessing Empagliflozin in bulk drug and in the pharmaceutical dosage form. Methods: The proposed method employs a Reverse Phase Shim Pack C18 column (250 mm × 4.6 mm id; 5 µm) using a mobile phase comprising of acetonitrile and water in the ratio of 60:40 v/v flushed at a flow rate of 1 ml/min. The eluents were monitored at 223 nm. Results: Empagliflozin was eluted at a retention time of 5.417 min and established a co-relation co-efficient (R2>0.999) over a concentration ranging from 0.0495-100µg/ml. Percentage recovery was obtained between 98-102% which indicated that the method is accurate. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were found at 0.0125µg/ml and 0.0495µg/ml, respectively. Conclusion: An RP-HPLC method which was relatively simple, accurate, rapid and precise was developed and its validation was performed for the quantitative analysis of empagliflozin in bulk and tablet dosage form (10 and 25 mg) in accordance to International Conference of Harmonization (ICH) Q2 (R1) guidelines. The proposed method may aid in routinely analyzing empagliflozin in pharmaceuticals.

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