scholarly journals Validation of assay method of nifedipine in tablets by liquid chromatography

2017 ◽  
Author(s):  
L. S. Lohoyda
Keyword(s):  
Liquid Chromatography ◽  
Quantitative Determination ◽  
High Performance ◽  
Hplc Method ◽  
Assay Method ◽  
Liquid Chromatograph ◽  
System A ◽  
Validation Of Methods ◽  
Validation Parameters

The aim of this study was the validation of methods of quantitative determination of nifedipine in  tablets by liquid chromatography. The chromatographic analysis was performed on nifedipine liquid chromatograph Agilent 1290 Infinity II LC System. A validation of methods of quantitative determination of nifedipine by high performance liquid chromatography tablets was performed. It was established that the method proves the requirements of the State Pharmacopoeia of Ukraine for the main validation parameters: specificity, accuracy, linearity, robasnist. The results obtained in this study clearly indicate that the developed HPLC method is fast, economical, simple, accurate and suitable for determination of nifedipine in medicines.

Validation of assay method of cardiazole by highly efficient liquid chromatography

2020 ◽  
Vol 26 (4) ◽  
pp. 80-90
Author(s):  
I.V. Drapak ◽  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Quantitative Determination ◽  
Analytical Method ◽  
High Performance ◽  
Antioxidant Properties ◽  
Stability Study ◽  
Assay Method ◽  
Validation Parameters

Aim. Validation of the method of quantitative determination of Cardiazole substance by high-performing liquid chromatography technique. Materials and Methods. The object of the study was the [3-allyl-4-(41-methoxyphenyl)-3H-thiazol-2-ylidene]-(32-trifluoromethylphenyl)-amine hydrobromide (Cardiazole) which possesses cardioprotective, anti-inflammatory, analgesic, hypolipidemic, antihypoxic, and antioxidant properties. The compound is patented and involved in the development plan of "Farmak" pharmaceutical company for further preclinical studies workflow. High-performance liquid chromatography was used for the quantitative determination of the Cardiazole substance. Validation of the proposed methodology was performed in accordance with the requirements of the State and European Pharmacopoeias requirements. The obtained data were analyzed using Analyst 1.5.2., as well as Statistica 10.0 and Microsoft Excel software. Results and Discussions. The high-performance liquid chromatography analytical method for the quantitative determination of Cardiazole substance was validated based on the main parameters according to the pharmacopeia requirements. The specificity of the technique was confirmed by comparing the chromatograms of the comparison solution, the test solution, and the blank solution. The linearity parameters are set over the entire range of the analyzed Cardiazole concentrations. The parameters of the correctness of the 9 prepared test solutions within the range of the analytical method application have met the following criteria: requirements for statistical and practical insignificance. The study of the parameters of intra-laboratory precision of 3 tests of the same sample was carried out by two analysts on different days during one week using different measuring ware. Thus, compliance with the criteria was confirmed. The obtained results of the experimental determining of the validation characteristics confirmed the correctness of the technique while reproduced in other laboratories. The results of the stability study showed: for optimal chromatography conditions it is necessary to use a freshly prepared solution of Cardiazole (within 24 hours). Conclusions. The evaluation of the validation parameters of the method of quantitative determination of Cardiazole by high-performance liquid chromatography was carried out. It was shown that the presented method of analysis of Cardiazole meets the requirements for specificity, linearity, accuracy, precision, and stability. The validated analytical method for the quantitative determination of Cardiazole by high-performance liquid chromatography can be used for standardization of the Cardiazole substance, as well as for studying the pharmacokinetics and pharmacodynamics, bioequivalence, and pharmaceutical development of dosage forms. Keywords: validation parameters, Cardiazole, high-performance liquid chromatography

scholarly journals ДОСЛІДЖЕННЯ ВАЛІДАЦІЙНИХ ХАРАКТЕРИСТИК МЕТОДИКИ КІЛЬКІСНОГО ВИЗНАЧЕННЯ ПАРАЦЕТАМОЛУ ТА ЙОГО ОСНОВНОЇ ДОМІШКИ В РЕКТАЛЬНИХ СУПОЗИТОРІЯХ

2021 ◽  
Vol 146 (3) ◽  
pp. 139-154
Author(s):  
О. О. Салій ◽  
Г. І. Кузьміна ◽  
Л. А. Фуклева ◽  
В. В. Манацюк
Keyword(s):  
Liquid Chromatography ◽  
Quantitative Determination ◽  
High Performance ◽  
Signal To Noise Ratio ◽  
Statistical Processing ◽  
Cost Effective ◽  
Hplc Method ◽  
Uv Detector ◽  
Main Impurity

Еxploration of validation characteristicsof the method for the quantitative determination of paracetamol and its main impurity 4-aminophenol in rectal suppositories by spectrophotometry (UV) and high performance liquid chromatography (HPLC). Spectrophotometric measurements were carried out on a UV VIS Lambda 35 spectrophotometer (Perkin Elmer, USA) in cuvettes l = 1 cm. We used a Waters 2695 liquid chromatography with a Waters 2489 UV-detector, as well as a Nucleosil C18 chromatographic column with a size of 250 × 4.6 mm, filled with octadecylsilyl sorbent with a particle size of 10 microns. We used reagents: purified water, which was obtained from the Milli Q plant, manufactured by Millipore Corporation (Germany), sodium hydroxide Sigma-Aldrich, cat. № 06203, sodium 1-butanesulfonate Sigma-Aldrich, cat. № 19022-10G-F; ethanol 96%, methanol Sigma-Aldrich (purity 99.9%), formic acid Sigma-Aldrich, cat. № 33015. Validation characteristics were confirmed as specificity, correctness, precision. The total predicted uncertainty of the analytical method for quantitative determination and the limit of quantitative determination of the main impurity of paracetamol, at which the signal-to-noise ratio is fulfilled, is 10% of the initial concentration of the reference solution (0.5 μg / ml). Confirmed linearity for quantitative determination of paracetamol content in the range of 80 to 120% of the nominal value. Statistical processing of experimental data was carried out; the correlation coefficient of the linear dependence (r) between the entered and found values for the quantitative determination of paracetamol is > 0.990, which indicates the correctness of the method. Methods for the quantitative determination of paracetamol and its main impurity in suppositories have been developed and validated. The method for quantitative determination of paracetamol in suppositories is significantly simpler for routine control of a batch of drugs and is cost-effective compared to the HPLC method. The obtained experimental results indicate that according to the studied validation characteristics, the technique is correct and can be reproduced in other laboratories.

scholarly journals DEVELOPMENT OF THE METHODOLOGY OF THE CHROMATOGRAPHIC DETERMINATION OF NIFEDIPINE IN MEDICINES

2017 ◽  
Vol 10 (3) ◽  
pp. 149 ◽  
Author(s):  
Liliya Logoyda ◽  
Dmytro Korobko ◽  
Serhii Kovalenko ◽  
Iryna Ivanusa
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Retention Time ◽  
High Performance ◽  
Chromatographic Determination ◽  
Hplc Method ◽  
Liquid Chromatograph ◽  
Relative Standard ◽  
Label Claim

ABSTRACTObjective: The aim was to develop a simple, rapid, less expensive, linear, precise, and accurate reverse phase high performance liquid chromatographymethod for determination of nifedipine in tablets.Methods: The chromatographic analysis of nifedipine was performed using liquid chromatograph Agilent 1290 Infinity II LC System. Selectedconditions were isocratic elution with binary mobile phase consisting of solution methanol and 0.1% trifluoroacetic acid (55:45). Detection wascarried out using spectrophotometric detector at 265 nm. The method was validated as per ICH guidelines.Results: The retention time for nifedipine by proposed high performance liquid chromatography (HPLC) method is observed as 3.5 minutes. Thecorrelation coefficients are 1.0000. The developed chromatographic method was found to be accurate with recovery 99.2-99.8% and was foundwithin the acceptance criteria (i.e. 98.0-102.0%) with acceptable % relative standard deviation of not more than 2% at each level. The assay results ofnifedipine in tablets by developed method are highly reproducible, reliable and are in good agreement with the label claim of the medicines (average99.62 %).Conclusion: Finally, it should be noted that a new simple, rapid, linear, precise, accurate HPLC method was developed and validated for thedetermination of nifedipine in medicines in accordance with the ICH guidelines. These results show the method are accurate, precise, sensitive,economic, and rugged. The proposed HPLC method is rapider (retention time is 3.5 minutes). This method can be useful for the routine analysis ofnifedipine in pharmaceutical dosage form.Keywords: Nifedipine, High-performance liquid chromatography, Validation, Linearity, Accuracy, Range of application.

scholarly journals RAPID AND ECONOMICAL QUANTITATIVE DETERMINATION OF SEVERAL ANTIHYPERTENSIVE AGENTS IN PRESENCE OF HYDROCHLOROTHIAZIDE BY ISOCRATIC REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY IN THEIR PHARMACEUTICAL PREPARATIONS

2017 ◽  
Vol 10 (12) ◽  
pp. 155
Author(s):  
Panchumarthy Ravisankar ◽  
Devala Rao G ◽  
Md Shaheem Sulthana ◽  
Supriya K ◽  
Mounika G ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Quantitative Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Control Analysis ◽  
Rp Hplc ◽  
Relative Standard

Objective: Objective of the present investigation is to develop a speedy isocratic reverse phase high-performance liquid chromatography (RP-HPLC) method for the separation and quantitative determination of 5 angiotensin II - receptor antagonists, namely, telmisartan, losartan, valsartan, olmesartan, irbesartan, and atenolol along with thiazide diuretics mostly hydrochlorothiazide (HCTZ).Methods: RP-HPLC method was evolved using Welchrom C18 column (4.6 × 250 mm, 5 μm) as a stationary phase with the mobile phase comprising a variety of phosphate buffer with pH-3.3 and acetonitrile in the proportion of 50:50 v/v. The mobile phase was pumped at a current rate of 1 mL/minute. The detection wavelength was carried out at 230 nm.Results: The total run time was 6 minutes and the elution window of only 3 minutes. The peaks were eluted with decorous resolution. The calibration curves were linear (r2=0.9998) in all cases. The percentage relative standard deviation (RSD%) was <2% and average recovery was above 99.95%. The method was validated specificity, precision, and accuracy. High recovery values and low RSD% prove that this method is very accurate and reproducible. The developed method was applied to the estimation of the above-said drugs in binary combinations from different manufacturers which were a good agreement with label claim.Conclusion: The important advantage of developed method was that the five individual drugs can be determined on a single chromatographic system without alteration in detection wavelength and mobile phase composition. This novel method was statistically validated as per ICH guidelines. The optimized method proved to be linear, accurate, and robust. Hence, the above said proposed method was found to be a rapid tool for the routine determination of the above-said drugs in alone or combination with HCTZ in quality control analysis without interference of excipients.

scholarly journals Development of HPLC method for determination of phenolic compounds on a core shell column by direct injection of wine samples

2020 ◽  
Vol 32 (2) ◽  
pp. 134-138
Author(s):  
Milica Atanacković Krstonošić ◽  
Jelena Cvejić Hogervorst ◽  
Mira Mikulić ◽  
Ljiljana Gojković-Bukarica
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Phenolic Compounds ◽  
High Performance ◽  
Direct Injection ◽  
Syringic Acid ◽  
Hplc Method ◽  
Core Shell ◽  
Validation Parameters

Phenolic compounds are frequently present in various natural products, and they can have different beneficial biological potentials. The most widely used method for determination of individual phenolic compounds is high-performance liquid chromatography (HPLC). In this paper, a method for simultaneous determination of 16 phenolic compounds (gallic acid, p-hydroxybenzoic acid, catechin, syringic acid, trans-cinnamic acid, hesperetin, naringenin, vanillic acid, benzoic acid, coumaric acid, resveratrol, chlorogenic acid, caffeic acid, rutin, quercetin, and kaempferol) on a core–shell column was developed. The separation method conducted on a standard ODS (250 mm) column was transferred to Poroshell column and optimized using non-ultra-high-performance liquid chromatography (UHPLC) apparatus. Phenolic compounds were separated fast and efficiently during 30-min analysis, and validation parameters were determined. The developed method was successfully applied on the analysis of phenolic content after direct injection of red wines from three different grape varieties.

Developing a High-performance Liquid Chromatography Method for Simultaneous Determination of Loratadine and its Metabolite Desloratadine in Human Plasma

2020 ◽  
Vol 20 (13) ◽  
pp. 1053-1059
Author(s):  
Mahmoud M. Sebaiy ◽  
Noha I. Ziedan
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Allergic Diseases ◽  
Reversed Phase ◽  
Hplc Method ◽  
H1 Receptor ◽  
Chromatography Method

Background: Allergic diseases are considered as the major burden on public health with increased prevalence globally. Histamine H1-receptor antagonists are the foremost commonly used drugs in the treatment of allergic disorders. The target drug in this study, loratadine, belongs to this class of drugs and its biometabolite desloratadine which is also a non-sedating H1 receptor antagonist with anti-histaminic activity being 2.5 to 4 times greater than loratadine. This study aimed to develop and validate a novel isocratic Reversed-phase High-Performance Liquid Chromatography (RP-HPLC) method for rapid and simultaneous separation and determination of loratadine and its metabolite, desloratadine in human plasma. Methods: The drug extraction method from plasma was based on protein precipitation technique. The separation was carried out on a Thermo Scientific BDS Hypersil C18 column (5μm, 250 x 4.60 mm) in a mobile phase of MeOH: 0.025M KH2PO4 adjusted to pH 3.50 using orthophosphoric acid (85: 15, v/v) at an ambient temperature. The flow rate was maintained at 1 mL/min and maximum absorption was measured using the PDA detector at 248 nm. Results: The retention times of loratadine and desloratadine in plasma samples were recorded to be 4.10 and 5.08 minutes, respectively, indicating a short analysis time. Limits of detection were found to be 1.80 and 1.97 ng/mL for loratadine and desloratadine, respectively, showing a high degree of sensitivity of the method. The method was then validated according to FDA guidelines for the determination of the two analytes in human plasma. Conclusion: The results obtained indicate that the proposed method is rapid, sensitive in the nanogram range, accurate, selective, robust and reproducible compared to other reported methods.

scholarly journals A Selective High-Performance Liquid Chromatography Method for the Determination of Reboxetine in Bulk Drug and Tablets

2006 ◽  
Vol 89 (6) ◽  
pp. 1552-1556
Author(s):  
ArmaĞan Önal ◽  
Olcay SaĞiri ◽  
S Müge Çetin ◽  
Sidika Toker
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Depressive Disorders ◽  
Degradation Products ◽  
Severe Depression ◽  
Hplc Method ◽  
Chromatography Method ◽  
Relative Standard

Abstract Reboxetine is used as a selective noradrenaline reuptake inhibitor for the treatment of major depressive disorders. It is effective in the treatment of severe depression and safer to use than traditional tricyclic antidepressants. In this study, a novel, simple, and rapid stability-indicating high-performance liquid chromatography (HPLC) method for reboxetine methansulfonate was successfully developed and validated for the assay of tablets. The method was used to quantify reboxetine in tablets; it employed a C18 column (150 4.6 mm id) with an isocratic mobile phase consisting of methanolphosphate buffer (pH 7, 0.02 M; 55 + 45, v/v) at a flow rate of 1.0 μmL/min. Reboxetine was detected by an ultraviolet detector at 277 nm. The retention time of reboxetine was about 4.5 min. The developed HPLC method was validated with respect to linearity, precision, sensitivity, accuracy, and selectivity. The method was linear over the concentration range 150 g/mL (r 0.9999). The limits of detection and the quantitation of reboxetine were 0.1 and 0.3 μg/mL, respectively. The relative standard deviation values for intraday and interday precision were 0.781.01 and 1.081.37%, respectively. Selectivity was validated by subjecting a stock solution of reboxetine to neutral, acid, and alkali hydrolysis, as well as oxidation, dry heat treatment, and photodegradation. The peaks of the degradation products did not interfere with the peak of reboxetine. The results indicated that the proposed method could be used in a stability assay. The proposed method was successfully applied to the determination of reboxetine in tablets. Excipients present in the tablets did not interfere with the analysis.

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