scholarly journals SIMULTANEOUS DETERMINATION OF TIGECYCLINE AND ITS POTENTIAL IMPURITIES BY A STABILITY-INDICATING RP-HPLC-UV DETECTION TECHNIQUE

2022 ◽  
pp. 75-82
Author(s):  
V. N. V. KISHORE ◽  
G. V. RAMANA
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Isocratic Elution ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Buffer Mixture ◽  
Bulk Drug ◽  
Tablet Dosage

Objective: Stability representing the RP-HPLC method was established for synchronized quantification of Tigecycline and its impurities. This method was confirmed for its applicability to both tablet dosage and bulk drug forms. Methods: Intended for an isocratic elution, a mobile phase containing methanol: 10 mmol Triethylamine Buffer mixture (75:25 v/v, pH 6.1) was used at 1 ml/min flow rate and Agilent ZORBAX Eclipse XDB C18 (250 mm × 4.6 mm, 5 μm) column. Results: At 231 nm as wavelength, high-pitched peaks of Tigecycline (Tig) and its impurities (1and2) were detected at 6.55, 8.73 and 4.87 min correspondingly. The linearity of tigecycline and its impurities (impurity-1 and 2 and) were estimated with ranging from 75–450 µg/ml for Tigecycline and 1–6 µg/ml for both impurity 1 and 2. The corresponding recognition limits (LOD and LOQ) of the tigecycline and its impurities were originated to be (1.37,0.047 and 0.071 µg/ml) and (4.15, 0.143 and 0.126 µg/ml). Conclusion: The technique was effectively stretched for stability signifying studies under different stress conditions. Justification of the method was done as per the current ICH guidelines.

scholarly journals Validated RP-HPLC Method for the Determination of Buspirone in Pharmaceutical Formulations

2011 ◽  
Vol 2011 ◽  
pp. 1-3 ◽  
Author(s):  
M. V. Basaveswara Rao ◽  
A. V. D. Nagendrakumar ◽  
Sushanta Maiti ◽  
Guttikonda Raja
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Isocratic Elution ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Precision And Accuracy ◽  
Tablet Dosage

A simple, selective, linear, precise, and accurate RP-HPLC method was developed and validated for the rapid assay of the Buspirone in tablet dosage form. Isocratic elution at a flow rate of 1.0 mL/min was employed on a symmetry C18 (250×4.6 mm, 5 μm in particle size) at ambient temperature. The mobile phase consisted of water : acetonitrile : methanol 45 : 35 : 20(V/V). The UV detection wavelength was 210 nm, and 20 μL sample was injected. The retention time for the Buspirone was 7.057 min. The percentage RSD for precision and accuracy of the method was found to be less than 2%. The method was validated as per the ICH guidelines. The method can be successfully applied for the routine analysis of Buspirone in tablet dosage form.

scholarly journals A Validated RP-HPLC Method for the Estimation of Pizotifen in Pharmaceutical Dosage Form

2012 ◽  
Vol 2012 ◽  
pp. 1-5 ◽  
Author(s):  
M. V. Basaveswara Rao ◽  
A. V. D Nagendrakumar ◽  
Sushanta Maiti ◽  
N. Chandrasekhar
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Isocratic Elution ◽  
Pharmaceutical Dosage Form ◽  
Reliable Determination ◽  
Rp Hplc ◽  
Ich Guidelines

A simple, selective, linear, precise, and accurate RP-HPLC method was developed and validated for rapid assay of Pizotifen in pharmaceutical dosage form. Isocratic elution at a flow rate of 1.0 mL/min was employed on Chromosil C18 (250 mm × 4.6 mm, 5 μm) column at ambient temperature. The mobile phase consists of methanol : acetonitrile in the ratio of 10 : 90 v/v. The UV detection wavelength was 230 nm, and 20 μL sample was injected. The retention time for Pizotifen was 2.019 min. The percent RSD for accuracy of the method was found to be 0.2603%. The method was validated as per the ICH guidelines. The method can be successfully applied for routine analysis of Pizotifen in the rapid and reliable determination of Pizotifen in pharmaceutical dosage form.

scholarly journals Stability indicating RP-HPLC method for the estimation of flucloxacillin sodium in a tablet dosage form

2020 ◽  
Vol 1 (4) ◽  
pp. 95-100
Author(s):  
Sonalika Patro ◽  
S. Harshith Kumar ◽  
M. Barath kumar ◽  
E. Masthaniah ◽  
K. Sairam ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Theoretical Plate ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
System Suitability ◽  
Precision Study ◽  
Tablet Dosage

A Simple, accurate and precise method was developed and validated for the determination of flucloxacillin sodium in its tablet dosage form. The separation was eluted on xterra c18 column (4.6x150mm, 5micron) using a mixture of octane buffer and methanol as mobile phase in a ratio of (30:70) which was pumped through column at a flow rate of  1ml/min. Optimised wavelength for flucloxacillin was 237nm, the retention time was 2.305minutes and the percentage purity was found to be 98.14%. System suitability parameters such as theoretical plate and tailing factor for flucloxacillin sodium was found to be 2991.64 and 1.90 respectively, the proposed method was validated as per ICH guidelines (ICH, Q2 AND (R1)) the method was found to be linear at the concentration range of 20-100µg/ml and the correlation coefficient (r2) value was found to be 0.9994 percentage RSD for precision was 0.9% and percentage RSD for ruggedness was 0.5%. The precision study was precise, robust and repeatable. The LOD and LOQ values are 2.98 and 9.98 respectively. Hence the suggested RP-HPLC method can be used for routine analysis for flucloxacillin sodium in tablet dosage form.

scholarly journals Validated RP-HPLC Method for the Determination of Ivabradine Hydrochloride in Pharmaceutical Formulation

2017 ◽  
Vol 9 (05) ◽  
Author(s):  
MD. Muzaffar -ur- Rehman1 ◽  
G. Nagamallika
Keyword(s):  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Bulk Drug

A simple, rapid, precise, and accurate RP-HPLC method for the estimation of Ivabradine Hydrochloride an anti-anginal agent, both as a bulk drug and in pharmaceutical formulation was developed. The chromatographic separation was achieved on a Thermosil C18 150 × 4.5 mm, 5μm column by using a mobile phase containing a mixture of methanol and phosphate buffer pH 6.5 in the ratio of 65:35 % v/v at a flow rate of 1ml/min and at an ambient temperature. The detection was monitored at a wavelength of 265nm. A clear chromatographic peak was identified with the retention time of 4.36 min and tailing factor of 1.23. The developed method was validated according to ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The method shows a good linear relationship with correlation co-efficient of more than 0.992 in the concentration range of 30μg-150μg. The method showed mean % Recovery of 100.4% and %RSD for repeatability and intermediate precision was less than 2%. The proposed method can be used successfully for the quantitative determination of Ivabradine HCL in pharmaceutical dosage forms.

Development and Validation of Stability Indicating RP-HPLC Method for Estimation of Voriconazole in Bulk Drug

2010 ◽  
Vol 3 (2) ◽  
pp. 978-986
Author(s):  
Wamorkar V V ◽  
C S Ramaa ◽  
Manjunath S Y ◽  
V Malla Reddy
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Good Resolution ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Bulk Drug ◽  
Development And Validation ◽  
Different Levels

RP-HPLC method has been developed and validated for the determination of voricaonazole in bulk drug. The developed method is found to be specific, reproducible, and stability indicating. The Hypersil, C18 (250 X 4.6 mm) 5μ column was used and mobile phase consisting of water:acetonitrile to achieve good resolution and retention of the analyte and its impurities. The detector linearity was established from concentrations ranging from 5-100 μg/ml. The method was tested at different levels of specificity and accuracy as per requirements given in ICH guidelines. The molecule was exposed to the stress conditions such as acid, base, oxidation, heat and light as per the recommendations of ICH guidelines. The method was proved to be robust with respect to changes in flow rate, mobile phase composition and allied columns. The proposed method is found to be sensitive, precise, rapid, reproducible, and offers good column life.

scholarly journals Stability indicating HPLC method for the simultaneous determination of dapagliflozin and saxagliptin in bulk and tablet dosage form

2018 ◽  
Vol 31 (1) ◽  
pp. 39-43 ◽  
Author(s):  
Thiyagarajan Deepan ◽  
Magharla Dasaratha Dhanaraju
Keyword(s):  
Particle Size ◽  
Flow Rate ◽  
Dosage Form ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Isocratic Elution ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Detection And Quantification

AbstractA simple, fast, and highly selective RP-HPLC method was developed for the determination of Dapagliflozin (DAP) and Saxagliptin (SAX) in API and tablet dosage form. The separation was done using a Xterra RP18 (4.6×150 mm, 5 μm particle size) column with Acetonitrile: water (60:40). The isocratic elution mode at a flow rate of 1 mL/min, and the analytes were measured at 248 nm. The retention time for DAP and SAX were about 2.091 and 3.249 min, respectively. Calibration curves were found to be linear in the ranges of 100-500 μg/ml for DAP and 50-250 μg/ml for SAX, with correlation coefficients of 0.9998. The detection and quantification values for DAP was 3.0 and 9.98 μg/ml and SAX was 3.02 and 10 μg/ml respectively.

scholarly journals Application of RP-HPLC method for the simultaneous determination of cetirizine in the presence of quinolones

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Hina Shamshad ◽  
Agha Zeeshan Mirza
Keyword(s):  
Human Serum ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Diclofenac Sodium ◽  
Internal Standard ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines

Abstract Background Present work describes a fast, simple, and sensitive procedure for the simultaneous determination of cetirizine in the presence of quinolones using diclofenac sodium as an internal standard. The present work was designed to analyze these compounds in pharmaceutical and clinical labs being economical for use. Results The mobile phase consisted of the simple composition of methanol, acetonitrile, and water in a ratio of 50:20:30 with a pH adjusted to 3.1 at a flow rate of 1 mL min−1. The UV detection was performed at 225 nm. The linearity was assessed over the range of 2.5–50 μg mL−1 for all drugs. The parameters such as accuracy, precision, linearity (>0.999), and sensitivity were satisfactory. Conclusion The method was equally applicable for formulation and human serum with recovery values between 95 and 105%. The results of the method were validated statistically according to ICH guidelines.

scholarly journals Optimization of RP-HPLC method with UV detection for determination of ursodeoxycholic acid in pharmaceutical formulations

2020 ◽  
Vol 66 (1) ◽  
pp. 85-90
Author(s):  
Zhaklina Poposka Svirkova ◽  
Zorica Arsova-Sarafinovska ◽  
Aleksandra Grozdanova
Keyword(s):  
Ursodeoxycholic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Pharmaceutical Formulations ◽  
Gradient Elution ◽  
Hplc Method ◽  
Uv Detection ◽  
Rp Hplc ◽  
Ich Guidelines

Due to the low absorptivity of bile acids, the aim of this study was to develop and validate a simple and sensitive HPLC/UV method for quantification of ursodeoxycholic acid (UDCA) in pharmaceutical formulations. Effective separation was achieved on C18 end–capped column, with gradient elution of a mobile phase composed of 0.001 M phosphate buffer (pH 2.8±0.5) – acetonitrile mix, at flow rate 1.5 mL min-1, UV detection at 200 nm and injection volumes were 50 µL. The proposed HPLC method was fully validated according to the ICH guidelines and it was found to be simple, accurate, precise and robust. Key words: ursodeoxycholic acid, HPLC/UV, pharmaceutical formulations, validation

RP-HPLC Method for Quantification of Etelcalcetide in Bulk and Parentral Dosage Form

2021 ◽  
pp. 5521-5526
Author(s):  
Krishna Kishore Adireddy ◽  
Srinivasa Rao Baratam ◽  
Nagarjuna Hari Pratap S.
Keyword(s):  
Flow Rate ◽  
Linear Response ◽  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Solution Stability ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
System Controller

A simple, rapid, accurate and precise RP-HPLC method was developed and validated for the determination of Etelcalcetide in bulk and parentral dosage form. Quantification of the drug was achieved on Shimadzu HPLC comprising of LC- 20 AD binary gradient pump, a variable wavelength programmable SPD-20A detector and SCL system controller. C18G column (250 mm x 4.6 mm, 5 μ) as stationary phase with mobile phase consisting of acetonitrile: methanol :water in the ratio of 25: 45 :30 v/v. The method showed a good linear response in the concentration range of 3.75-22.5 μg/ml with correlation coefficient of 0.9999. The flow rate was maintained at 1.0 ml/min and effluents were monitored at 238 nm. The retention time of etelcalcetide was 6.201 min. The method was statistically validated for accuracy, precision, linearity, ruggedness, robustness, solution stability, selectivity and sensitivity. The results obtained in the study were within the limits of ICH guidelines and hence this method can be used for the determination of etelcalcetide in bulk and parentral dosage form.

scholarly journals Box-Behnken Assisted Validation and Optimization of an RP-HPLC Method for Simultaneous Determination of Domperidone and Lansoprazole

Separations ◽  
2021 ◽  
Vol 8 (1) ◽  
pp. 5
Author(s):  
Mohd Afzal ◽  
Mohd. Muddassir ◽  
Abdullah Alarifi ◽  
Mohammed Tahir Ansari
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Box Behnken Design ◽  
Rp Hplc ◽  
System Suitability ◽  
Method Optimization ◽  
Key Variables

A highly specific, accurate, and simple RP-HPLC technique was developed for the real-time quantification of domperidone (DOMP) and lansoprazole (LANS) in commercial formulations. Chromatographic studies were performed using a Luna C8(2), 5 μm, 100Å, column (250 × 4.6 mm, Phenomenex) with a mobile phase composed of acetonitrile/2 mM ammonium acetate (51:49 v/v), pH 6.7. The flow rate was 1 mL·min−1 with UV detection at 289 nm. Linearity was observed within the range of 4–36 µg·mL−1 for domperidone and 2–18 µg·mL−1 for lansoprazole. Method optimization was achieved using Box-Behnken design software, in which three key variables were examined, namely, the flow rate (A), the composition of the mobile phase (B), and the pH (C). The retention time (Y1 and Y3) and the peak area (Y2 and Y4) were taken as the response parameters. We observed that slight alterations in the mobile phase and the flow rate influenced the outcome, whereas the pH exerted no effect. Method validation featured various ICH parameters including linearity, limit of detection (LOD), accuracy, precision, ruggedness, robustness, stability, and system suitability. This method is potentially useful for the analysis of commercial formulations and laboratory preparations.

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