scholarly journals A modified RP-HPLC method for the determination of the pKa values of synthesized β-hydroxy-β-arylalkanoic acids

2018 ◽  
Vol 83 (7-8) ◽  
pp. 875-883
Author(s):  
Jelena Savic ◽  
Sanda Dilber ◽  
Zorica Vujic ◽  
Sote Vladimirov ◽  
Jasmina Brboric
Keyword(s):  
Pure Water ◽  
Volume Ratio ◽  
Hplc Method ◽  
Poor Correlation ◽  
Pka Values ◽  
Rp Hplc ◽  
Mobile Phases ◽  
Wide Range ◽  
Buffer Mixture ◽  
Sigmoidal Curve

The pKa values of twelve ?-hydroxy-?-arylalkanoic acids and ibuprofen were determined using a modified RP-HPLC method. The stationary phase was octadecyl modified (C-18) silica gel, and the mobile phases were mixtures of methanol and one of ten different buffers (60:40 volume ratio). The mean retention time of each compound was plotted against the pH of each of the ten used mobile phases. The inflection point of the obtained sigmoidal curve represents the s w pKa of a compound. Using s w pKa in previously established equations for the specific methanol/buffer mixture, the w w pKa values (in pure water) were calculated. The obtained w w pKa values for the synthesized compounds were in a range from 3.40 to 3.74, and the w w pKa for ibuprofen was 4.27. The Predicted pKa values for this type of compounds in the MarvinSketch 5.11.5. Program were in poor correlation with the experimental results, while in ACD/ /I-Labs pKa values were calculated as a wide range.

scholarly journals A new RP-HPLC method as an auxiliary tool for optimization of sample preparation procedures for tracing of PPCPs of different hydrophilicities

2021 ◽  
Vol 71 (2) ◽  
pp. 305-315
Author(s):  
Omar J. Portillo-Castillo ◽  
Rocío Castro-Ríos ◽  
Abelardo Chávez-Montes ◽  
Azucena González-Horta ◽  
Norma Cavazos-Rocha ◽  
...  
Keyword(s):  
Sample Preparation ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Suitable Alternative ◽  
Analytical Technique ◽  
Rp Hplc ◽  
Mobile Phases ◽  
Wide Range ◽  
Gradient Mode

AbstractRecently, pharmaceutical and personal care products (PPCPs) have received considerable attention because of their increasing use. Analysis of PPCPs presents a significant analytical challenge, with high-performance liquid chromatography (HPLC) in reversed-phase mode, as the most widely used analytical technique. To facilitate the optimization of the procedures that are applied in the early stages of sample preparation, a simple and fast HPLC method is proposed in this work for the separation of some PPCPs with a wide range of hydrophilicity. Two columns were evaluated (Atlantis dC18 and Discovery HS F5); as for mobile phases: a formate buffer (40 mmol L−1, pH 4) and methanol were tested in a gradient mode. The fluorinated column allowed better separation in a shorter time and better resolution for all analytes (Rs > 1). The proposed method delivered good performance for the tracing of PPCPs and is a suitable alternative to traditional C18-based HPLC methods.

scholarly journals Development and Validation of Stability-Indicating RP-HPLC Method for the Estimation of Lenalidomide and its Impurities in Oral Solid Dosage Form

2019 ◽  
Vol 35 (1) ◽  
pp. 140-149 ◽  
Author(s):  
Somana Siva Prasad ◽  
G. V. Krishna Mohan ◽  
A. Naga Babu
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Stability Robustness ◽  
Rp Hplc ◽  
Mobile Phases ◽  
Limit Of Quantitation ◽  
Successful Separation ◽  
Quality By Design Approach

In this study, a novel, simple and precise RP-HPLC method has been developed for the quantitative analysis of Lenalidomide (LLM) in pharmaceutical formulations using analytical quality by design approach. An X-bridge-C18 column (150 mm × 4.6 mm × 3.5 µ) with mobile phases containing a Potassium dihydrogen orthophosphate anhydrous buffer and methanol in the ratio of (90:10 v/v) and (35:65 v/v) are used for the estimation of LLM and its degradation products. The flow rate of 0.8 mL/min is maintained and all degradation studies are performed at 210 nm using photodiode array (PDA) detector. Method Validation is carried out according to International Council for Harmonisation (ICH) guidelines and the parameters namely; precision, accuracy, specificity, stability, robustness, linearity, limit of quantitation (LOQ) and limit of detection (LOD) are evaluated. The present developed RP-HPLC method shows the purity angle of peaks is less than their threshold angle, signifying that it to be suitable for stability studies. Hence, the developed method can be used for the successful separation of LLM and its impurities in the pharmaceutical dosage formulations.

scholarly journals Qualitative and quantitative evaluation of melittin in honeybee venom and drug products containing honeybee venom

2013 ◽  
Vol 57 (2) ◽  
pp. 37-44 ◽  
Author(s):  
Ghasem Haghi ◽  
Alireza Hatami ◽  
Mehdi Mehran
Keyword(s):  
High Performance ◽  
Pure Water ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Honeybee Venom ◽  
Drug Products ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Main Component

Abstract A reverse-phase high-performance liquid chromatographic (RP -HPLC ) method was developed and validated for the analysis of honeybee venom samples and drug products containing honeybee venom. The validation parameters were linearity, sensitivity, precision, and recovery. Melittin is the main component of honeybee venom was extracted with pure water, and then evaluated by RP -HPLC with a photodiode array (PDA ) detector. Separation of the samples was achieved on a Europa Protein C18 column with linear gradient elution of acetonitrile and 0.4% phosphoric acid at 25°C. There was a flow rate of 1 mL/min. Detection was set at 220 nm. Limits of detection (LOD ) and quantification (LO Q) for melittin were 1.1 and 3.2 μg/mL, respectively. The amount of melittin in honeybee venom samples ranged from 21.9 to 66.4 %.

scholarly journals Development and Validation of Simple, Rapid and Sensitive High- Performance Liquid Chromatographic Method for the Determination of Butenafine Hydrochloride

2020 ◽  
pp. 116-125
Author(s):  
Mohammad Javed Ansari ◽  
Mohammed Muqtader Ahmed ◽  
Md. Khalid Anwer ◽  
Mohammed F. Aldawsari ◽  
Saad M. Al Shahrani ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Linear Regression Analysis ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Least Square ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Relative Standard ◽  
Wide Range

Aims: The current paper reports a simple, rapid, sensitive, accurate, and precise Reverse-phase high performance liquid chromatography (RP-HPLC) method with wide range of estimation to determine butenafine hydrochloride in nanosponges. This method has been validated as per ICH norms. Study Design:  Experimental design with influence of variables such as mobile phase composition, flow rate, temperature and wavelength on the chromatographic peaks. Place and Duration of Study: Department of Pharmaceutics, College of Pharmacy, Prince Sattam Bin Abdulaziz University, Al-Kharj, Saudi Arabia between Jan 2020 and March 2020. Methodology: Separation was achieved by utilizing the most commonly used reverse phase column (C-18, 5 μm, 150 mm x 4.6 mm) set at 30ºC and quantified by UV detection at 280 nm after isocratic elution from a mobile phase (70:30 v/v of methanol: phosphate buffer pH 3.0) flowing at 1 ml/min. Results: A sharp and symmetrical peak was observed at 4.08 ± 0.01 minutes. The low variation in peak area and retention time (1.12% and 0.29%, respectively) and a high number of theoretical plates (>2000) indicated this method’s efficiency and suitability. The least square linear regression analysis (Y = 9265.5 X + 1961.4) showed excellent correlation (r2 = 0.999 ± 0.0003) between concentration and peak area of butenafine hydrochloride through a wide concentration range of 1–50 µg/ml. The limits of detection and quantification (LOD and LOQ) were 0.18 µg/ml and 0.57 µg/ml, respectively. The assay or determinations were accurate, precise and reproducible with mean accuracy and mean relative standard deviation of precision of 101.53 ± 0.43% and 0.51 ± 0.11% respectively. Conclusion: The developed RP-HPLC method was simple, sensitive, reproducible with wide range of estimation of butenafine hydrochloride in the nanosponges. The proposed method could be used for the analysis of butenafine hydrochloride in the conventional pharmaceutical formulations such as tablets, syrup, creams including novel formulations such as nanoparticles, nanosponges, nanoemulsions. The proposed method overcomes the specificity, sensitivity and reproducibility related issues of ultraviolet-visible spectroscopy.

Method Development and Validation of Degradation Studies of Lenalidomide by RP-HPLC

2021 ◽  
pp. 4281-4286
Author(s):  
Punna Venkateshwarlu ◽  
Mehul M. Patel
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Mobile Phase Flow Rate ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
System Suitability ◽  
Wide Range

A simple, accurate, RP HPLC method was developed by this study determination of lenalidomide. This method is developed by Shimadzu LC -2010 HT by using C18 (250 X 4.6 X mm X 5µ) column in solvents Phosphate buffer: Acetonitrile (55:45) v/v as mobile phase and the temperature was maintained at 25°C. The mobile phase flow rate 1ml/min was pumped and sample wavelength was detected at 242nm by ultraviolet -visible spectrophotometer. The retention time was found 2.5 min. The number of theoretical plates and tailing factor for lenalidomide was observed 16199.817 (NLT 2000) and 1.128 (NMT 2). The method was validated for analytical standards such as linearity, accuracy, precision, system suitability and robustness. LOD and LOQ values obtained from regression of lenalidomide 0.058 and 0.174µg/ml. The regression equation of validated method for lenalidomide is Y=5223x+183075. In wide range of 25 to 150 (µg/ml) the linearity was observed. The method was validated and a recovery study indicates accuracy of this method. The Retention time less compared to established methods. The method was validated by determining its accuracy, precision and system suitability. The results of the study showed that the proposed RP-HPLC method is simple, rapid, precise and accurate, which is useful for the routine determination of Lenalidomide in bulk drug and in its pharmaceutical dosage forms.

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 Development of Isocratic RP-HPLC Method for Separation and Quantification of L-Citrulline and L-Arginine in Watermelons

2018 ◽  
Vol 2018 ◽  
pp. 1-9 ◽  
Author(s):  
Rasdin Ridwan ◽  
Hairil Rashmizal Abdul Razak ◽  
Mohd Ilham Adenan ◽  
Wan Mazlina Md Saad
Keyword(s):  
Amino Acid ◽  
Acid Content ◽  
Citrullus Lanatus ◽  
Amino Acid Content ◽  
Hplc Method ◽  
Efficient Separation ◽  
Rp Hplc ◽  
Mobile Phases ◽  
Freeze Dried ◽  
Arginine Concentration

Watermelons(Citrullus lanatus)are known to have sufficient amino acid content. In this study, watermelons grown and consumed in Malaysia were investigated for their amino acid content, L-citrulline and L-arginine, by the isocratic RP-HPLC method. Flesh and rind watermelons were juiced, and freeze-dried samples were used for separation and quantification of L-citrulline and L-arginine. Three different mobile phases, 0.7% H3P04, 0.1% H3P04, and 0.7% H3P04 : ACN (90 : 10), were tested on two different columns using Zorbax Eclipse XDB-C18and Gemini C18with a flow rate of 0.5 mL/min and a detection wavelength at 195 nm. Efficient separation with reproducible resolution of L-citrulline and L-arginine was achieved using 0.1% H3P04on the Gemini C18column. The method was validated and good linearity of L-citrulline and L-arginine was obtained withR2= 0.9956,y=0.1664x+2.4142andR2=0.9912,y=0.4100x+3.4850, respectively. L-citrulline content showed the highest concentration in red watermelon of flesh and rind juice extract (43.81 mg/g and 45.02 mg/g), whereas L-arginine concentration was lower than L-citrulline, ranging from 3.39 to 11.14 mg/g. The isocratic RP-HPLC method with 0.1% H3P04on the Gemini C18column proved to be efficient for separation and quantification of L-citrulline and L-arginine in watermelons.

Method Development and Validation for Estimation of related Substances in Tilorone Dihydrochloride using RP¬-HPLC

2021 ◽  
pp. 3319-3324
Author(s):  
M. Zeba Baktiyar ◽  
B. Mohammed Ishaq ◽  
Siva Sanker Reddy L ◽  
Sreenivasulu M.
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Column Temperature ◽  
Related Substances ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Wide Range ◽  
Method Development And Validation ◽  
Development And Validation

A simple, precise and reproducible RP-HPLC method was developed for the estimation of related substances in tilorone dihydrochloride. Quantification was performed using a Zorbax SB-phenyl column (150 × 4.6mm, 5µ) with mobile phase A: 20mM potassium dihydro phosphate + 2ml of triethylamine, pH 2.30 and mobile phase B: acetonitrile, methanol and water 60: 20: 20% v/v. A gradient program was followed with a run time of 55 minutes at a flow rate of 1.0 ml/min. The column temperature was maintained at 40°C, the injection volume was 10 µl and the detection was performed at 269nm using a PDA detector. The retention time of Tilorone dihydrochloride was found to be 10.36 minutes. The proposed method has been validated according to the ICH guidelines for Linearity, Precision, Accuracy, LOD, and LOQ. The method was linear from 0.157 - 3.934μg/ml for standard, 0.153-3.820μg/ml and 0.166 - 4.140μg/ml for impurities, TLHC01 and TLHC02 respectively. The impurities TLHC01 and TLHC02 have been mapped in all stress conditions. The LOD and LOQ of TLHC01 were found at 1.757μg/ml and 5.857μg/ml and 1.919μg/ml and 6.396μg/ml respectively for TLHC02 respectively. Statistical analysis showed that the method was precision, reproducible, selective, specific and accurate for the analysis of Tilorone dihydrochloride and its impurities. The wide range of linearity, sensitivity, precision, short retention times and simple mobile phase have shown that the method is suitable for the routine quantification of mass impurities of tilorone hydrochloride and its dosage pharmaceutical forms with high precision and accuracy.

METHOD DEVELOPMENT AND VALIDATION OF RP-HPLC FOR THE SIMULTANEOUS ESTIMATION OF ESCITALOPRAM AND ETIZOLAM IN BULK AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (02) ◽  
pp. 50-56
Author(s):  
S. Vadrevu ◽  
◽  
K. Govindarao
Keyword(s):  
Dosage Forms ◽  
Hplc Method ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Good Resolution ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Mobile Phases

The developed RP-HPLC method allows rapid and precise determinations of escitalopram and etizolam in bulk and pharmaceutical dosage forms. The objective of the proposed method was to develop a simple and accurate method for the determination of escitalopram and etizolam by RP-HPLC method in pharmaceutical dosage forms & its stability indicative studies. A series of mobile phases were tried; among the various mobile phases , potassium dihydrogen phosphate buffer and dipotassium hydrogen phosphate 0.02 M, pH 3.0 : acetonitrile (20:80) is an ideal mobile phase, since it gave a good resolution and peak shapes with perfect optimization. The flow rate was optimized at less than 2 mL/min. The linearity and correlation coefficient of escitalopram and etizolam at 0-45μg/mL and 0-75μg/mL was found to be 0.998 & 0.998, respectively. The LOD was found to be 0.1 mg/mL and 0.3 mg/mL and LOQ was found to be 0.15 mg/mL and 0.45 mg/mL for escitalopram and etizolam, respectively, which represents that sensitivity of the method is high. The method was known to be accurate with the assay method. The % assay was found to be 100 % and 98%. The developed method showed a good accuracy and precision. The % RSD is for escitalopram and etizolam was found to be 1.50 and 1.22. This method shows good reproducibility of the results. Furthermore, this method was simple, sensitive, and accurate. Hence, the chromatographic method developed for escitalopram & eizolam can be effectively applied for routine analysis.

scholarly journals Method Development and Validation of Degradation Studies of Favipiravir by RP-HPLC

2021 ◽  
pp. 220-228
Author(s):  
. Shyamala ◽  
Dongamanti Ashok
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Mobile Phase Flow Rate ◽  
Rp Hplc ◽  
Wide Range ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Analytical Standards ◽  
Theoretical Plates

RP HPLC method was developed by this study estimation of favipiravir. This method is developed by Shimadzu LC -2010 HT by using a C18 (250 X 4.6 X mm X 5µ) column in solvents Water(OPA)+ACN  (60:40)v/v as mobile phase and the temperature was maintained at 25°C. The mobile phase flow rate of 1ml/min was pumped and sample wavelength was detected at 324 nm by ultraviolet -visible spectrophotometer. The Rt was found 4.453 min. The number of theoretical plates and tailing factor for favipiravir was observed 82651(NLT 2000) and 1.265 (NMT 2). The method was validated for analytical standards such as linearity, accuracy, precision, LOD, LOQ and robustness. LOD and LOQ values were calculated from regression of favipiravir 1.26 and 3.83 µg/ml.The regression equation of validated method for favipiravir is Y=253.5x+1881.In a wide range of 4 to 20 (µg/ml) the linearity was observed. Degradation methods were also performed.

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