scholarly journals Validation of an Oil-in-Water Microemulsion Liquid Chromatography Method for Analysis of Perindopril tert-Butylamine and Its Impurities

2011 ◽  
Vol 94 (3) ◽  
pp. 723-734 ◽  
Author(s):  
Marija Mašković ◽  
Yannis Dotsikas ◽  
Anđelija Malenović ◽  
Biljana Jančić-Stojanović ◽  
Darko Ivanović ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Method Validation ◽  
Dihydrogen Phosphate ◽  
Mobile Phase Flow Rate ◽  
Pharmaceutical Dosage Form ◽  
Validation Parameters ◽  
Tert Butylamine ◽  
Microemulsion Liquid Chromatography

Abstract This paper describes the development and validation of a microemulsion liquid chromatography (MELC) method for simultaneous determination of perindopril tert-butylamine and its impurities in bulk active substances and the pharmaceutical dosage form of tablets. An appropriate resolution with reasonable retention times was obtained for a microemulsion containing 0.24% (w/v) butyl acetate, 0.30% (w/v) ethyl acetate, 2% (w/v) sodium dodecyl sulfate, 7.75% (w/v) n-butanol, and 20.0 mM potassium dihydrogen phosphate, the pH of which was adjusted to 3.70 with 85% orthophosphoric acid. Separations were performed on a Nucleosil 120-5 butyl modified (C4), 250 × 4 mm, 5 μm particle size silica column at 40°C, with a mobile phase flow rate of 1.25 mL/min. UV detection was performed at 254 nm. The established method was subjected to method validation, and required validation parameters were defined. Robustness testing, an important part of method validation, was performed as well. Since robustness validation can be conducted using different experimental designs, the Plackett-Burman design was applied due to its possibility of testing many factors at the same time. The validated MELC method was found to be suitable for the simultaneous determination of perindopril tert-butylamine and its impurities in pharmaceuticals.

scholarly journals SIMULTANEOUS DETERMINATION OF METFORMIN, LINAGLIPTIN IN JENTADUETO AND METFORMIN, SAXAGLIPTIN IN KOMBIGLYZE BY LC-MS METHOD

2018 ◽  
Vol 10 (3) ◽  
pp. 110
Author(s):  
P. B.n. Prasad ◽  
K. Satyanarayana ◽  
G. Krishna Mohan
Keyword(s):  
Simultaneous Determination ◽  
Degradation Products ◽  
Spectrometric Method ◽  
Mass Spectrometric Method ◽  
Pharmaceutical Dosage Form ◽  
Economic Method ◽  
Validation Parameters ◽  
Acceptance Limits ◽  
Positive Ion

Objective: The objective of the present investigation was to develop a novel, simple and economic method for the determination of metformin (MET), linagliptin (LIN) and saxagliptin (SAX) in jentadueto and kombiglyze sample by employing the liquid chromatography and mass spectrometric method for estimation in bulk and pharmaceutical dosage form in presence of degradation products.Methods: The chromatographic separation was achieved by using the mobile phase composition of methanol and ammonium acetate buffer pH 4.5 (85:15 % v/v) on the Hypurity advance C-18 column at a flow rate of 0.5 ml/min. Ion signals m/z “130.10/70.10, 473.10/420.40 and 316.30/180.20” for metformin, linagliptin and saxagliptin respectively measured in positive ion mode. The detailed validation of the method was performed as per ICH guidelines.Results: The results of all validation parameters found within acceptance limits. The linearity of the drugs was found to be in the concentration range of 50–5000 ng/ml for all the drugs. Accuracy of the drugs was found to be from 94-102% and precision was found 4.67% RSD for all three drugs. The validated method was employed for the determination of drugs in the formulation and also determined the drugs in the presence of degradation products under stress conditions.Conclusion: The method was developed and validated as per guidelines. Hence, this method can be used for the simultaneous determination of metformin, linagliptin and metformin, saxagliptin in bulk and combined dosage forms.

Simultaneous determination of metformin and glimepride in pharmaceutical dosage form by reverse-phase liquid chromatography

2005 ◽  
Vol 28 (16) ◽  
pp. 2076-2079 ◽  
Author(s):  
Bhaskar Laxmanrao Kolte ◽  
Bharat Baburao Raut ◽  
Adwait Anant Deo ◽  
Manoj Anil Bagool ◽  
Devanand Baburao Shinde
Keyword(s):  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Dosage Form ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Reverse Phase Liquid Chromatography ◽  
Phase Liquid

scholarly journals Analysis of Flavonoids and Iridoids in Vitex Negundo by HPLC-PDA and Method Validation

2013 ◽  
Vol 8 (9) ◽  
pp. 1934578X1300800
Author(s):  
Somendu K. Roy ◽  
Khemraj Bairwa ◽  
Jagdeep Grover ◽  
Amit Srivastava ◽  
Sanjay M. Jachak
Keyword(s):  
Quality Control ◽  
Simultaneous Determination ◽  
Method Validation ◽  
Hplc Method ◽  
Vitex Negundo ◽  
Good Recovery ◽  
Bioactive Constituents ◽  
Ich Guidelines ◽  
Validation Parameters

The leaves of Vitex negundo have been reported to contain various bioactive constituents including iridoids and flavonoids. This is the first report on the simultaneous determination of iridoids and flavonoids by HPLC in three different samples of V. negundo leaves collected from three regions of India. Separation of iridoids and flavonoids was accomplished by HPLC and further elaborated for their quantification in V. negundo leaves using a C-18 column with detection at 254 and 330 nm, respectively. The developed HPLC method showed good linearity (r2≥0.999), high precision (RSD<5%) and a good recovery (99.3–103.0%) of the compounds. All the validation parameters of the developed HPLC were found to be within the permissible limits according to the ICH guidelines. The developed method was robust, accurate and reliable for the quality control of V. negundo leaves.

Validated Stability-Indicating RP-HPLC Method for Simultaneous Determination of Clorsulon and Ivermectin Employing Plackett-Burman Experimental Design for Robustness Testing

2016 ◽  
Vol 99 (2) ◽  
pp. 571-578 ◽  
Author(s):  
Ahmed S Saad ◽  
Nahla S Ismail ◽  
Marwa Soliman ◽  
Hala E Zaazaa
Keyword(s):  
Experimental Design ◽  
Simultaneous Determination ◽  
Degradation Products ◽  
Hplc Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Sodium Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating

Abstract A sensitive and highly selective stability-indicating gradient HPLC method was developed and validated for simultaneous determination of clorsulon (CLO) and ivermectin (IVM) in the presence of their degradation products. The drugs were subjected to different stress conditions, including acid and alkaline hydrolysis, oxidative, thermal, and photolytic forced degradation. The robustness of the proposed method was assessed using the Plackett-Burman experimental design, the factors affecting system performance were defined, and nonsignificant intervals for the significant factors were determined. The separation was carried out on a ZORBAX SB phenyl analytical column (250 × 4.6 mm id, 5 μm particle size), with gradient elution utilizing 10 mM sodium dihydrogen phosphate and acetonitrile as mobile phase. UV detection was performed for CLO and IVM at 254 nm over a concentration range of 4–140 and 5–50 μg/mL, respectively, with mean percentage recoveries of 99.90 ± 1.30 and 98.59 ± 1.16%, respectively. The proposed method was successfully applied to a pharmaceutical dosage form containing the investigated drugs. The results were statistically compared with the official HPLC methods, and no significant differences were found.

Simultaneous Determination of Sulfonamides in Honey by Liquid Chromatography

1992 ◽  
Vol 75 (5) ◽  
pp. 786-789 ◽  
Author(s):  
Masakazu Horie ◽  
Koichi Saito ◽  
Norihide Nose ◽  
Hiroyuki Nakazawa
Keyword(s):  
Liquid Chromatography ◽  
Sodium Chloride ◽  
Simultaneous Determination ◽  
Rapid Method ◽  
Mobile Phase ◽  
Dihydrogen Phosphate ◽  
Sodium Dihydrogen Phosphate ◽  
Domestic Products ◽  
Sodium Dihydrogen

Abstract A simple and rapid method using liquid chromatography (LC) for the simultaneous determination of 10 sulfonamides (sulfathiazole, sulfadimethoxine, sulfamonomethoxine, sulfadiazine, sulfamerazine, sulfadimidine [sulfamethazine], sulfamethoxazole, sulfamethoxypyridazine, sulfachloropyridazine, and sulfaquinoxaline) in honey has been developed. Samples were dissolved in 30% sodium chloride and then extracted with dichloromethane. The extracts were cleaned up on a Sep-Pak Florisil cartridge. The LC separation was performed on a LiChrosphere RP-18e column (250 x 4.0 mm id) with 0.05M sodium dihydrogen phosphate-acetonitrile (2 +1) as the mobile phase; the drugs were detected at 275 nm with 0.04 AUFS. The calibration graphs were rectilinear from 1 to 40 ng for each drug. The recoveries at the level of 0.5 µg/g were 62.1-90.2%, and the detection limits were 0.05 µg/g for each drug. Sulfamonomethoxine was found in 2 samples of domestic products at levels of 0.23 and 0.83 µg/g.

scholarly journals Development and Validation of Stability Indicating Reverse Phase High Performace Liquid Chromatography Method for the Determination of Umeclidinium and Vilanterol in Pharmaceutical Dosage Form

2021 ◽  
pp. 208-219
Author(s):  
Ahsaana Hamsa ◽  
K. Praseetha ◽  
K. P. Dijin Raj ◽  
T. V. Ashira ◽  
O. V. Athira ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Relative Standard ◽  
Validation Parameters ◽  
The Stability

A Sensitive, fast, linear and accurate liquid chromatography technique was developed for the simultaneous determination of Umeclidinium and Vilanterol in Powder dosage form. The estimation was carried out using Phenomenex C18 column (150 × 4.6 mm, 5μ) with ammonium acetate: acetonitrile taken in the ratio 60:40 as mobile phase and pumped at a flow rate of 0.9 ml/min at 300C. Detection wavelength selected was 245 nm. Retention times of Umeclidinium and Vilanterol were found to be 2.219 min and 2.794 min. The method was validated in terms of linearity, precision, accuracy, limit of detection, limit of quantification as per International council for harmonization guidelines. Degradation studies performed indicated the stability of the drug. All of these analytical validation parameters were evaluated, and the percent relative standard deviations were calculated, indicating the method's suitability for determination of Umeclidinium and Vilanterol in pharmaceutical dosage form.

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