A COMPARISON OF HPLC ANALYSIS OF NITRATE IN SOILS WITH THE PHENOLDISULFONIC ACID AND HYDRAZINE SULFATE METHODS

1986 ◽  
Vol 66 (1) ◽  
pp. 151-157 ◽  
Author(s):  
T. C. KUCHNICKI ◽  
G. R. B. WEBSTER
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Chemical Compositions ◽  
Hydrazine Sulfate ◽  
Reverse Phase ◽  
Silver Sulfate ◽  
Water Ph ◽  
Nitrate Analysis ◽  
Physical And Chemical

Six Manitoba soils of varying physical and chemical compositions were used to determine the efficiency of nitrate analysis by high-performance liquid chromatography (HPLC). The nitrate was extracted with distilled water and the extract was analyzed with a reverse phase column using a mobile phase of 1:1 methanol-water, pH 3.0. In five soils, the HPLC method of nitrate analysis resulted in near 100% recovery of added nitrate. An average 90.2% recovery was obtained with the hydrazine sulfate method using sodium bicarbonate, pH 8.5, as the soil extractant. Variable recoveries were obtained with the phenoldisulfonic acid method using a silver sulfate-copper sulfate extractant. Key words: HPLC, nitrate analysis, soil

Analytical Method of Gliotoxin Content by HPLC

2012 ◽  
Vol 581-582 ◽  
pp. 46-49
Author(s):  
Xin Qing Zhang ◽  
Ze Ping Xu ◽  
Chuan Lun Yang ◽  
Jian Ping Wang ◽  
Zheng Wei
Keyword(s):  
High Performance Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Mixed Solution ◽  
Determination Method ◽  
Reverse Phase ◽  
Average Recovery ◽  
Reliable Basis

Objective: To establish a determination method for gliotoxin. Methods: Reverse-phase high performance liquid chromatography (HPLC) method was used：the column was Inertsil ODS-SP; detection wavelength set at 254 nm; mixed solution of menthol and water（50:50）was used as the mobile phase with flow rate of 1.0 mL/min. Results: The regression equation of gliotoxin content was y = 9E–08x–0.003. The linear range was 0.5-2.5mg/mL and the average recovery was 99.22%. Conclusion: This method is simple, effective and suitable for analysis of the gliotoxin. A reliable basis was provided for the determination of gliotoxin.

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.

scholarly journals Reverse-phase High-Performance Liquid Chromatography Method Development and Validation for Estimation of Glimepiride in Bulk and Tablet Dosage Form

2020 ◽  
Vol 11 (02) ◽  
pp. 296-302
Author(s):  
Aseem Kumar ◽  
Anil Kumar Sharma ◽  
Rohit Dutt
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Development And Validation

The present work demonstrates a simple, rapid, precise, specific, and sensitive reverse-phase high-performance liquid chromatography (RP-HPLC) method for analyzing glimepiride in pure and tablet forms. The present method was developed using a C18 column 150 × 4.6 mm, with 5 μm, and packing L1 maintained at a temperature of 30°C. The mobile phase was prepared by dissolving 0.5 gram of monobasic sodium phosphate in 500 mL of distilled water, pH of the solution adjusted to 2.1 to 2.7 with 10% phosphoric acid, and added 500 mL of acetonitrile. The mobile phase was pumped in the highperformance liquid chromatography (HPLC) system at a flow rate of 1 mL/min, and separation was carried out at 228 nm, using an ultraviolet (UV) detector. The chromatographic separation was achieved with peak retention time (RT) at about 9.30 minutes, and the method was found to be linear over a concentration range of 40 to 140 μg/mL. The specificity of the method represented no interference of the excipients during the analysis, and stability testing after 24 hours also showed that the method is suitable and specific. The accuracy was between 99.93 to 99.96%, with limit of detection (LOD) and limit of quantitation (LOQ) being 0.354 μg/mL, 1.18 μg/mL, respectively. Satisfactory results were found for precision and robustness parameters during the development and validation stage for the analytical method. The proposed method was also adopted for the analysis of glimepiride tablets to improve the overall quality control. Using this method, symmetric peak shape was obtained with reasonable retention time. The retention time of glimepiride for six repetitions is 9.3 ± 0.1 minutes; the run time is 21 minutes. The proposed RP-HPLC method is a modification of the United States Pharmacopeia (USP) method, and it was found to be valid for glimepiride within concentration ranges 40 to 140 μg/mL, using C18 analytical columns, and isocratic elution with UV detection, and at 1 mL/min of flow rate.

scholarly journals Development and validation of RP-HPLC method for the estimation of omeprazole in bulk and capsule dosage forms

2012 ◽  
Vol 1 (11) ◽  
pp. 366-369 ◽  
Author(s):  
Kalakonda Sri Nataraj ◽  
Mohammad Badrud Duza ◽  
Kalyani Pragallapati ◽  
Dussa Kiran Kumar
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Accurate Method ◽  
Pharmaceutical Journal ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Development And Validation

A method for the determination of omeprazole in bulk and capsule dosage form by reverse phase high performance liquid chromatography has been developed. This is a simple, rapid, precise and an accurate method. The method was developed on a Novapak C18, (250 x 4.6 mm, 5µ) column using phosphate buffer (pH 7.4) and acetonitrile in the ratio of 60:40, v/v as a mobile phase which was pumped at a flow rate of 1.0 ml/min and detection was done at 302 nm. The retention time of the drug was found to be 7.71 min. The method was validated for accuracy, precision, linearity, specificity, robustness. The linearity was observed in the range of 20-60 ppm. The results of recovery studies indicated that the method was accurate. Hence the developed method was found to be suitable for the estimation of omeprazole in bulk and capsule dosage forms.DOI: http://dx.doi.org/10.3329/icpj.v1i11.12062 International Current Pharmaceutical Journal 2012, 1(11): 366-369

scholarly journals A Novel Reverse Phase HPLC Method for the Quantification of Potential Genotoxic Impurities in Doripenem Monohydrate: A Broad-Spectrum Carbapenem Antibiotic Drug

2021 ◽  
Vol 33 (6) ◽  
pp. 1325-1330
Author(s):  
Sudhakar Yerra ◽  
P.N. Kishore Babu ◽  
B. Sreenivasulu ◽  
Hemant Kumar Sharma ◽  
K. Mohana Naidu ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Side Chain ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Antibiotic Drug ◽  
Genotoxic Impurities

A novel sensitive gradient reverse phase high performance liquid chromatographic (RP-HPLC) method has been developed and validated for the quantification of potential genotoxic impurities in doripenem monohydrate (DORIBAX) drug substance, namely mono-p-nitrobenzyl malonate, 1β-methyl bicyclic ketoester, desilylated β-keto ester, 1β-methyldiazoazetidinone, deprotected doripenem side chain, N-protected mercapto alcohol, protected doripenem and doripenem side chain. The analysis performed on Alliance Waters e2695 separation module on C18 (250 × 4.6) mm, 5 μm (make: Inertsil) column, oven temperature maintained at 40 ºC and UV detection at 270 nm. The separation was accomplished using buffer (pH 6.0 ± 0.05) and acetonitrile in the ratio of 98:2 v/v as mobile phase-A and acetonitrile as mobile phase-B, flow rate: 1.0 mL/min and injection volume: 50 μL. The proposed method was validated as per ICH guidelines in terms of limit of detection (LOD), limit of quantification (LOQ), linearity, precision, accuracy and specificity.

High Performance Liquid Chroma tographic Analysis of Dicofol Acaricide

1980 ◽  
Vol 63 (6) ◽  
pp. 1296-1299
Author(s):  
Alan M Rothman
Keyword(s):  
Acetic Acid ◽  
High Resolution ◽  
Mobile Phase ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
High Performance Liquid Chroma ◽  
Hplc Method ◽  
Reverse Phase ◽  
In Series ◽  
Liquid Chromatographic

Abstract Kelthane Technical, a dicofol acaricide marketed by Rohm and Haas Co., and 18 impurity components can be resolved by a new reverse phase high performance liquid chromatographic (HPLC) method using a methanol-water-acetic acid (75+25+0.2) mobile phase, a high resolution C8 column in series with a short Cl8 s guard column, and detection at 254 nm. Relative elution volumes: and relative sensitivities for all known Kelthane Technical components are reported. This HPLC method has few co-elution problems, can be performed on a basic HPLC system, avoids the thermal degradation of Kelthane experienced in the previously established gas-liquid chromatographic (GLC) procedures, and can detect all impurity components to at least 0.1% level.

scholarly journals A NOVEL ANALYTICAL METHOD FOR SIMULTANEOUS QUANTIFICATION OF DAPAGLIFLOZIN AND SITAGLIPTIN BY REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

2021 ◽  
Vol 10 (3) ◽  
pp. 2861-2865
Author(s):  
Ajay Gupta
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
High Performance ◽  
Potassium Phosphate ◽  
Cost Effective ◽  
Gradient Elution ◽  
Hplc Method ◽  
Reverse Phase ◽  
Simultaneous Quantification ◽  
Validation Parameters

The Reverse phase HPLC method was developed for simultaneous determination of Dapagliflozin and Sitagliptin in single analytical method. Chromatographic separation was achieved on a Hypersil BDS C18 (250mmx4.6mm, 5µm) column applying an gradient elution based on potassium phosphate monobasic buffer pH (3.0) as mobile phase A while methanol and acetonitrile in the ratio of (60:40 v/v) as a mobile phase B with gradient program Time/Mobile phase A%/Mobile phase B% is as 0 min./55/45, 3 min./55/45, 9 min./20/80, 13 min.20/80, 15 min./55/45, 20 min./55/45. Validation parameters specificity, linearity, accuracy, precision and robustness have been observed to be desirable over the concentration ranges of 50-150 µg/ml for Dapagliflozin and Sitagliptin respectively. All the variables have been studied to optimize the chromatographic conditions. The optimized approach verified through validation and confirmed to be the intended purpose for the quality control of the mentioned drugs, as per ICH guidelines. For simultaneous quantification of Dapagliflozin and Sitagliptin, the developed method was found to be genuinely exact precise, accurate, linear, fast, and cost effective.

Development, Validation and Application of HPLC Method for Metformin in Rabbit Plasma

2019 ◽  
Vol 15 (6) ◽  
pp. 574-579
Author(s):  
Muhammad Ubaid ◽  
Mahmood Ahmad ◽  
Farhan Ahmad Khan ◽  
Ghulam Murtaza
Keyword(s):  
Flow Rate ◽  
Present Method ◽  
Mobile Phase ◽  
Hplc Method ◽  
Plasma Samples ◽  
Rabbit Plasma ◽  
Uv Detector ◽  
Reverse Phase ◽  
T Values ◽  
Pharmacokinetic Evaluation

Objective:This study was aimed at conducting a pharmacokinetic evaluation of metformin in rabbit plasma samples using rapid and sensitive HPLC method and UV detection.Methods:Acetonitrile was used for protein precipitation in the preparation of plasma samples. Reverse phase chromatography technique with silica gel column (250 mm × 4.6 mm, 5 μm) at 30°was used for the separation purpose. Methanol and phosphate buffer (pH 3.2) mixture was used as a mobile phase with flow rate 0.8 ml/min. The wavelength of UV detector was adjusted at 240 nm.Results:The calibration curve was linear in a range of 0.1-1 µg/ml with R² = 0.9982. The precision (RSD, %) values were less than 2%, whereas, accuracy of method was higher than 92.37 %. The percentage recovery values ranged between 90.14 % and 94.97 %. LOD and LOQ values were 25 ng/ml and 60 ng/ml, respectively. Cmax and AUC0-t values were found to be 1154.67 ± 243.37 ng/ml and 7281.83 ± 210.84 ng/ml.h, respectively after treating rabbits with a formulation containing 250 mg metformin.Conclusion:Based on the above findings, it can be concluded that present method is simple, precise, rapid, accurate and specific and thus, can be efficiently used for the pharmacokinetic study of metformin.

scholarly journals METHOD VALIDATION OF RIFAMPICIN ANALYSIS IN HUMAN PLASMA AND ITS APPLICATION IN BIOEQUIVALENCE STUDY

2019 ◽  
pp. 296-303
Author(s):  
ENDANG LUKITANINGSIH ◽  
FATHUL JANNAH ◽  
RATNA BUDHI PEBRIANA ◽  
RATNA DEWI PUSPITA ◽  
TAUFIQUROHMAN . ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Bioequivalence Study ◽  
Hplc Method ◽  
Coefficient Of Determination ◽  
European Medicines Agency ◽  
Pharmacokinetic Profiles ◽  
Relative Standard ◽  
Precision And Accuracy ◽  
Bioequivalence Test

Objective: This research aims to validate the method for rifampicin analysis in plasma by using High-Performance Liquid Chromatography (HPLC) that can be used to study the bioequivalence of a generic tablet of rifampicin 450 mg “X” marketed in Indonesia. Methods: Bioequivalence test was analysed using HPLC equipped with UV-Vis detector at 377 nm. The mobile phase used was acetonitrile-phosphate buffer pH 6.8 (45:55) delivered at a flow rate of 1.5 ml/min. Bioequivalence test was conducted on a limited number of subjects (n=8). The subjects were divided into two groups randomly. The pharmacokinetic profiles of the test tablet and reference tablet were statistically calculated using SPSS program to see the test tablet and reference tablet were bioequivalence or not. Results: The developed HPLC method for rifampicin analysis in plasma was sufficiently valid based on the International Conference on Harmonization (ICH) and European Medicines Agency (EMA) guideline, with precision and accuracy values were % Relative Standard Deviation (% RSD = 1.40–13.04) and % Recovery (86.24–102.13), respectively. Meanwhile, the method was linear over studied concentration (0.05 to 10.26 µg/ml) with a coefficient of determination (R2) = 0.9984. The method also had good stability and sensitivity. The result of statistical calculation showed that the generic rifampicin tablet X was bioequivalence toward the reference tablet Rimactan 450 mg. Conclusion: The test rifampicin tablet that was, the generic tablet “X” was bioequivalence toward the reference rifampicin tablet “Rimactan”.

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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