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 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 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 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.

Development of reverse phase-high performance liquid chromatography (RP-HPLC) method for determination of selected antihypertensive active flavonoids (rutin, myricetin, quercetin, and kaempferol) in medicinal plants found in Botswana

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Katso Binang ◽  
David T. Takuwa
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Medicinal Plants ◽  
High Performance ◽  
Zingiber Officinale ◽  
Hplc Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Lippia Javanica

Abstract The aim of the study was to develop a rapid, efficient, and cheap chromatographic method for determining four selected antihypertensive active flavonoid compounds in medicinal plants in Botswana. The determination of rutin, quercetin, and kaempferol in selected medicinal plants was conducted in less than 6 min using the developed reverse phase-high performance liquid chromatography (RP-HPLC) method with a 2.7 µm Ascentis C18 express column (150 × 4.60 mm i.d) at 340, 360, and 368 nm detection wavelengths and mobile phase of methanol and 0.068% of formic acid solution in isocratic elution. Validation results showed good selectivity, linearity (r 2 > 0.99), high percentage recoveries (90.2–104.7%), and precision (% RSD < 2) for n = 3, confirming suitability of the method for determination of the investigated flavonoids in Zingiber officinale (ginger). Application of the developed RP-HPLC method was performed in selected medicinal plants (Lippia javanica ) (mosukujane), Myrothanmus flabellious (galalatshwene), and Elephantorrhiza elephantina (mositsana) used to manage hypertension by herbalists in Botswana. M. flabellious a very commonly used plant for managing hypertension was found to contain highest amounts of rutin and myricetin, whereas nothing was detected for E. elephantina.

Assay and Dermatokinetics of Tetrahydrocurcumin Lipidic Nanostructures Using Reverse Phase-High Performance Liquid Chromatography

2021 ◽  
Vol 09 ◽  
Author(s):  
Priyanka Narula ◽  
Komal Saini ◽  
Megha Saini ◽  
Dinesh Singla ◽  
Anurag Singh Chauhan ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Quantitative Estimation ◽  
Healing Process ◽  
Entrapment Efficiency ◽  
Hplc Method ◽  
Reverse Phase ◽  
Chromatography Method ◽  
Rp Hplc

Background: Envisaging the poor solubility (56ng/ml) and permeability of tetrahydrocurcumin (THCC), it was formulated into lipidic nanostructures to enhance its bioavailability upon topical application to promote the healing process for skin inflammatory disorders. Lack of literature on suitable method for determining THCC per se and nanoformulations prompted us to develop a RP-HPLC method to detect the drug in its nanostructures and in pig ear skin post dermatokinetics. Objective: The present investigation aimed to develop a simple, precise and RP-HPLC method for the quantitative estimation of THCC in prepared lipidic nanostructures, its ointment and in skin homogenate obtained post dermatokinetic study. Method: THCC encapsulated nanostructures and ointment were formulated using modified emulsification method and embedded into an ointment base to enhance its spreadability and improve patient compliance. A fast and sensitive reverse phase high performance liquid chromatography method was developed using a Hypersil BDS reverse phase C18 column (4.6 mm × 250 mm, 5 μm) with mobile phase comprising tetrahydrofuran (THF) and 1 mgmL-1 citric acid (4:6), at a flow rate of 1.0 mLmin−1 with a run time of 20 min. Result: THCC nanostructures were successfully prepared using spontaneous microemulsification method. THCC was detected at 282 nm and revealed two peaks which were attributed to the keto-enol tautomerism in the molecule with retention times of 6.23 min and 11.06 min respectively. The assay of THCC in nanostructures and ointment was found to be 98.30% and 99.98% with entrapment efficiency 77.00±2.74 %. The dermatokinetic studies revealed sufficient release of THCC from its ointment up till 24 hr with a concentration of 1382 μgcm-2, for causing a therapeutic effect. Conclusion: The method was found to be reproducible and robust as shown by low coefficient of variation and a constant analyte/IS ratio. It was successfully employed for the estimation of THCC assay in nanostructures and it’s ointment and dermatokinetic analysis in skin.

scholarly journals ESTIMATION OF AMLODIPINE BESYLATE AND IRBESARTAN IN PHARMACEUTICAL FORMULATION BY RP-HPLC WITH FORCED DEGRADATION STUDIES

2019 ◽  
pp. 159-167 ◽  
Author(s):  
T Hemant Kumar ◽  
CH. ASHA ◽  
D. GOWRI SANKAR
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Forced Degradation ◽  
Amlodipine Besylate ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Liquid Chromatographic

Objective: To develop and validate a simple, specific, accurate, precise and sensitive reverse phase high performance liquid chromatographic (RP-HPLC) method with forced degradation studies for the simultaneous estimation of amlodipine besylate and irbesartan in the pharmaceutical formulation. Methods: The chromatographic separation of the two drugs were achieved using Enable C 18G column (250 ×4.6 mm; 5 µm) in isocratic mode with mobile phase consisting of sodium acetate buffer (pH 4.0) and acetonitrile (30:70, % v/v) with a flow rate of 0.6 ml/min. Ultraviolet(UV) detection was carried out at 238 nm. The proposed method was validated for linearity, range, accuracy, precision, robustness, limit of detection (LOD) and limit of quantification (LOQ). The tablet formulation was subjected to stress conditions of degradation including acidic, alkaline, oxidative, thermal and photolysis. Results: The retention time for amlodipine besylate and irbesartan were found to be 5.512 and 6.321 min respectively. Linearity was observed over a concentration range 4-32 µg/ml for amlodipine besylate (r2 =0.9999) and 10-70 µg/ml for Irbesartan (r2 =0.9998). The % relative standard deviation (RSD) for Intraday and Interday precision was found to be 0.436 and 0.699 for amlodipine besylate and 0.435 and 0.30 for irbesartan. Amlodipine besylate shown stability towards acidic and thermal whereas in basic, oxidative and photolytic it shown less stability in which it degraded to more extent. Irbesartan shown stability towards thermal conditions whereas in remaining conditions it degrades to more extent especially in oxidative conditions. Conclusion: The developed reverse phase high performance liquid chromatographic (RP-HPLC) method was also found to be simple, precise and sensitive for the simultaneous determination of amlodipine besylate and irbesartan in the tablet dosage form.

scholarly journals DEVELOPMENT AND VALIDATION OF REVERSE PHASE-HIGH PERFORMANCE LIQUID CHROMATOGRAPHY ASSAY METHOD FOR ESTIMATION OF FENOFIBRATE IN TABLET DOSAGE FORM PREPARED USING CRYSTALLO-CO-AGGLOMERATES OF THE DRUG

2021 ◽  
Vol 19 (1) ◽  
pp. 19-28
Author(s):  
SANTOSH GANDHI ◽  
MANGESH BHALEKAR ◽  
RAVINA MUTHA
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Linear Regression Analysis ◽  
Hplc Method ◽  
Assay Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Specificity And Sensitivity ◽  
Tablet Dosage

The aim of the present study was to develop a simple isocratic reverse phase-high performance liquid chromatography (RP-HPLC) method and validate for the determination of fenofibrate in tablet dosage forms. RP-HPLC method was developed using Hi Q Sil C18 (250 cm × 4.6 mm, 5 μm) and mobile phase comprising 1 mM ammonium acetate buffer: Acetonitrile (10:90 v/v) at a flow rate of 1.0 mL/min. The detection was carried out at 290 nm. The retention time was found to be 6.15 ± 0.03 min. Validation of the method was performed for precision, accuracy, linearity, robustness, specificity and sensitivity to conform to the International Conference on Harmonization (ICH) guidelines. The data of linear regression analysis indicated a good linear response in the concentration range of 5 μg/mL–30 μg/mL with correlation co-efficient (R2) of 0.997. The developed method was found to be simple, sensitive, accurate and repeatable for assay of tablets of fenofibrate prepared using crystallo-co-agglomerates of the drug.

scholarly journals RP-HPLC Method Development and Validation of Synthesized Codrug in Combination with Indomethacin, Paracetamol, and Famotidine

2020 ◽  
Vol 2020 ◽  
pp. 1-9 ◽  
Author(s):  
Mohyeddin Assali ◽  
Murad Abualhasan ◽  
Nihal Zohud ◽  
Noura Ghazal
Keyword(s):  
High Performance ◽  
Method Development ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Active Ingredients ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Relative Standard ◽  
Hplc Method Development

Background. Indomethacin is considered a potent nonsteroidal anti-inflammatory drug that could be combined with Paracetamol to have superior and synergist activity to manage pain and inflammation. To reduce the gastric side effect, they could be combined with Famotidine. Methodology. A codrug of Indomethacin and Paracetamol was synthesized and combined in solution with Famotidine. The quantification of the pharmaceutically active ingredients is pivotal in the development of pharmaceutical formulations. Therefore, a novel reverse-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated according to the International Council for Harmonization (ICH) Q2R1 guidelines. A reverse phase C18 column with a mobile phase acetonitrile: sodium acetate buffer 60 : 40 at a flow rate of 1.4 mL/min and pH 5 was utilized. Results. The developed method showed good separation of the four tested drugs with a linear range of 0.01–0.1 mg/mL (R2 > 0.99). The LODs for FAM, PAR, IND, and codrug were 3.076 × 10−9, 3.868 × 10−10, 1.066 × 10−9, and 4.402 × 10−9 mg/mL respectively. While the LOQs were 9.322 × 10−9, 1.172 × 10−10, 3.232 × 10−9, and 1.334 × 10−8 mg/mL, respectively. Furthermore, the method was precise, accurate, selective, and robust with values of relative standard deviation (RSD) less than 2%. Moreover, the developed method was applied to study the in vitro hydrolysis and conversion of codrug into Indomethacin and Paracetamol. Conclusion. The codrug of Indomethacin and Paracetamol was successfully synthesized for the first time. Moreover, the developed analytical method, to our knowledge, is the first of its kind to simultaneously quantify four solutions containing the following active ingredients of codrug, Indomethacin, Paracetamol, and Famotidine mixture with added pharmaceutical inactive ingredients in one HPLC run.

scholarly journals METHOD DEVELOPMENT AND VALIDATION OF EPROSARTAN MESYLATE AND ITS IMPURITIES USING REVERSE PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2016 ◽  
Vol 8 (4) ◽  
pp. 49 ◽  
Author(s):  
O. S. S. Chandana ◽  
D. Sathis Kumar ◽  
R. Ravichandra Babu
Keyword(s):  
High Performance ◽  
Method Development ◽  
Hplc Method ◽  
Reverse Phase ◽  
Related Substances ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
The Mean ◽  
Development And Validation

Objective: Our main objective is to develop an accurate and precise RP-HPLC method for the determination of Eprosartan Mesylate and its impurities. Methods: A Develosil ODS UG-5; (150 × 4.6) mm; 5 µm column was used for the Separation of drugs by a mobile phase consisting of Buffer and Acetonitrile mixture in the gradient proportion. The flow rate maintained was 0.8 ml/min and the wavelength used for detection was 235 nm.Results: The linearity was observed in the range of 0.025-50µg/ml of spiked impurities in Eprosartan Mesylate, impurity 1 and impurity 2 with a correlation coefficient of 0.99927, 0.99910 and 0.99934 respectively. The mean percentage recoveries for LOQ, 50%, 80%, 100%, 150% and 200% accuracy were found to be 101.5±1.51, 107.0±1.7, 104.6±0.4, 102.8±0.36, 101.7±0.26 and 101.3±0.15 respectively for impurities in Eprosartan Mesylate, impurity 1 and impurity 2. Linearity, accuracy, precision and robustness parameters for the suggested method were estimated for validation.Conclusion: The developed method is uncomplicated, accurate, sensitive and precise for the determination of related substances in the Eprosartan Mesylate. The satisfying % recoveries and low % RSD Values confirmed the suitability of the developed method for the usual analysis of Eprosartan mesylate in pharmaceuticals.

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