scholarly journals Toxicokinetic Study of a Gastroprotective Dose of Capsaicin by HPLC-FLD Method

Molecules ◽  
2019 ◽  
Vol 24 (15) ◽  
pp. 2848 ◽  
Author(s):  
Mónika Kuzma ◽  
Krisztina Fodor ◽  
Attila Almási ◽  
Gyula Mózsik ◽  
Tibor Past ◽  
...  
Keyword(s):  
General Circulation ◽  
High Performance ◽  
Limit Of Detection ◽  
Development Program ◽  
Mucosal Damage ◽  
Gastric Mucosal Damage ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Inflammatory Drugs ◽  
Anti Inflammatory

Background: A low dose of capsaicin and its natural homologs and analogs (capsaicinoids) have shown to prevent development of gastric mucosal damage of alcohol and non-steroid anti-inflammatory drugs. Based on this experimental observation, a drug development program has been initiated to develop per os applicable capsaicin containing drugs to eliminate gastrointestinal damage caused by non-steroid anti-inflammatory drugs. Methods: As a part of this program, a sensitive and selective reverse-phase high-performance liquid chromatography-based method with fluorescence detection has been developed for quantification of capsaicin and dihydrocapsaicin in experimental dog’s plasma. Results: The method was evaluated for a number of validation characteristics (selectivity, repeatability, and intermediate precision, LOD, LOQ, and calibration range). The limit of detection (LOD) was 2 ng/mL and the limit of quantification (LOQ) was 10 ng/mL for both capsaicin and dihydrocapsaicin. The method was used for analysis of capsaicin and dihydrocapsaicin in the plasma samples obtained after per os administration of low doses (0.1, 0.3, and 0.9 mg/kg bw) of Capsaicin Natural (USP 29) to the experimental animals. Conclusions: The obtained results indicated that the administered capsaicinoids did not reach the general circulation.

scholarly journals STABILITY INDICATING VALIDATED HPLC METHOD FOR THE DETERMINATION OF ZANUBRUTINIB IN BULK AND PHARMACEUTICAL DOSAGE FORM

2020 ◽  
pp. 159-162
Author(s):  
M. VIJAYA KUMARI ◽  
CH. BALASEKHAR REDDY
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Reversed Phase ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Form ◽  
Acceptable Limit ◽  
Relative Standard

Objective: An accurate, rapid economical and straight forward, reliable assay technique was evolved and showed for the evaluation of zanubrutinib using reversed-phase high-performance liquid chromatography. Methods: In the proposed method, efficient chromatographic separation was achieved applying acetonitrile and 0.1% orthophosphoric acid (50:50 v/v) as a mobile phase with a flow of 1 ml/min and the wavelength was observed at 220 nm. Chromatography was administered isocratically at ambient temperature and run time was approximately 6 min and the retention time (Rt) was observed as 4.358 min. Results: The method was justified as per ICH guidelines. System suitability parameters were studied by injecting the quality six fold and results were well under acceptance criteria. Linearity study was administered between 10% and 150% levels, regression coefficient value was observed as 0.999. Limit of detection and limit of quantification were observed as 0.02 μg/ml and 0.2 μg/ml, respectively. Precision was found to be 0.74 for repeatability and 0.68 for intermediate precision. Recovery of the drug was found to be 98–102%, indicates that the recovery is in the acceptable limit. Validation results were found to be satisfactory and the method applicable for bulk and formulation analysis. Hence, it was evident that the proposed method was said to be suitable for regular analysis and quality control of pharmaceutical preparations. Conclusion: The validation results were in good agreement with the acceptable limit. Relative standard deviation values which are <2.0% indicating the accuracy and precision of this method. Assay of retail formulation was administered and found to be 100.24% was present using the above method. Stress conditions of degradation in acidic, alkaline, peroxide, and thermal were studied. This developed method showed reliable, precise, accurate results under optimized conditions.

scholarly journals Development of the simultaneous analysis of choline salicylate, lidocaine hydrochloride and preservatives in a new dental gel by HPLC method

Chemija ◽  
2021 ◽  
Vol 32 (2) ◽  
Author(s):  
Yuliia Maslii ◽  
Ivan Bezruk ◽  
Anna Materiienko ◽  
Olena Ruban ◽  
Liudas Ivanauskas ◽  
...  
Keyword(s):  
Quantitative Determination ◽  
High Performance ◽  
Limit Of Detection ◽  
Phosphate Buffer Solution ◽  
Hplc Method ◽  
Lidocaine Hydrochloride ◽  
Buffer Solution ◽  
Limit Of Quantification ◽  
Intermediate Precision

A new high-performance liquid chromatography (HPLC) method for the simultaneous quantitative determination of active pharmaceutical substances and preservatives in a new dental medication has been developed. The optimization of HPLC method parameters was done through studies of a mobile phase composition and a detection wavelength. Our developing method uses an ACE C18 column (250 × 4.6 mm, 5 µm) and a gradient mode for separation with the acetonitrile and phosphate buffer solution (adjusted to pH 3.0) as mobile phases. The flow rate is 1 ml/ min, and the detection was set at 260 nm (DAD). The method was evaluated according to the ICH guidelines and the State Pharmacopoeia of Ukraine in terms of specificity, accuracy, linearity and precision (repeatability and intermediate precision). The limit of detection and the limit of quantification were also calculated. The developed method was put in place for the analysis of a combined dental gel to a quantitative determination of the APIs (choline salicylate, lidocaine hydrochloride) and preservatives (methylparaben, propylparaben).

scholarly journals Validation of an HPLC method for the determination of amino acids in feed

2013 ◽  
Vol 78 (6) ◽  
pp. 839-850 ◽  
Author(s):  
Igor Jajic ◽  
Sasa Krstovic ◽  
Dragan Glamocic ◽  
Sandra Jaksic ◽  
Biljana Abramovic
Keyword(s):  
Amino Acids ◽  
High Performance ◽  
Limit Of Detection ◽  
High Specificity ◽  
Hplc Method ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Chromatography Method

The subject of this study is the validation of a high-performance liquid chromatography method for the analysis of amino acids in feed. The contents of amino acids were determined in maize, soybean, soybean meal, as well as in their mixtures enriched with different amounts of methionine, threonine and lysine. The method involves the acid hydrolysis of the sample (6 h at 150?C), automated derivatisation of amino acids with the aid of o-phthaldialdehyde and 9-fluorenylmethyl chloroformate reagents, separation on the ZORBAX Eclipse-AAA column, and detection using a diode-array detector. The method is characterized by high specificity (the difference between the retention times of the feed samples and standard mixtures are below 1.7 %), wide linear range (from 10 to 1000 nmol cm-3, r2 = 0.9999), high accuracy (recovery 93.3-109.4 %), and the precision of the results (RSD below 4.14 % in case of repeatability and below 4.57 % in the case of intermediate precision). The limit of detection and the limit of quantification are in the range 0.004-1.258 ?g cm-3 and 0.011-5.272 ?g cm-3, respectively. The results demonstrate that the procedure can be used as a method for the determination of the composition of primary amino acids of feed proteins.

scholarly journals Simultaneous determination of some illegal antihypertensive and diuretic drugs in traditional herbal preparations by HPLC-DAD

2021 ◽  
Vol 4 (2) ◽  
pp. 99-108
Author(s):  
Hung Pham Van ◽  
Son Tran Cao ◽  
Kieu Anh Nguyen Thi ◽  
◽  
◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Local Market ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Herbal Products ◽  
Herbal Preparations ◽  
Diuretic Drugs

A simple, stable, and specific high-performance liquid chromatography coupled with a&nbsp;DAD detector (HPLC-DAD) method has been developed and validated for the simultaneous&nbsp;determination of amlodipine, felodipine, furosemide, nifedipine, and spironolactone in&nbsp;traditional herbal products. The analytes were extracted in acetonitrile: water (50 : 50, v/v) with&nbsp;help of the ultrasonic. The separation of analytes was performed in an Apollo C18 column (250&nbsp;&times; 4.6 mm; 5 &mu;m) and a mobile phase consisting of mixture acetonitrile: 0.1% phosphoric acid in&nbsp;gradient elution. The analyzed drugs were detected at 238 nm. The method was validated according&nbsp;to the AOAC International guidelines concerning specificity, linearity, precision (repeatability,&nbsp;intermediate precision), accuracy, limit of detection (LOD), and limit of quantification (LOQ).&nbsp;The method can detect the studied drugs at the concentration of 0.66 to 1.25 &mu;g/g for dry&nbsp;samples and 0.10 to 0.24 &mu;g/mL for liquid samples. The method was successfully applied in the&nbsp;analysis of 17 samples in the local market. No samples were found positive for the substances to&nbsp;be analyzed.

scholarly journals DETERMINATION OF MEFENAMIC ACID IN A TOPICAL EMULGEL BY A VALIDATED HPLC METHOD

2019 ◽  
pp. 86-90
Author(s):  
APICHART ATIPAIRIN ◽  
SOMCHAI SAWATDEE
Keyword(s):  
Mefenamic Acid ◽  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Gelling Agent ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Intermediate Precision

Objective: The present study is aimed to develop and validate a simple, precise and accurate high-performance liquid chromatography (HPLC) method, according to ASEAN guideline for the validation of the analytical procedure, for the determination of mefenamic acid in a topical emulgel preparation. Methods: An emulgel of 1 % mefenamic acid was prepared using carbopol 940 as a gelling agent and cremophor EL as an emulsifying agent. It was diluted with ethanol to make a sample concentration of 200 mg/ml. The method used a C18 column (5 µm; 250 x 4.6 mm) with the mobile phase, consisting of acetonitrile, acetic acid, and water in a ratio of 75:1:24. The column was maintained at 25 °C. The flow rate was 1 ml/min and the injection volume was 10 ml. The peak response was monitored by UV at 282 nm. It was validated for specificity, range, linearity, precision, accuracy, limit of detection (LOD) and limit of quantification (LOQ). In addition, forced degradation (hydrolysis, oxidation and dry heat) was performed to determine the capability of the proposed method to analyze the chemical stability of the drug samples during storage. Results: The method was specific to the drug while other excipients did not interfere with the quantitation of mefenamic acid. It was linear in the concentration range of 1.29 to 806 mg/ml. LOD and LOQ were 4.88 and 14.78 mg/ml, respectively. Accuracy of the method was demonstrated by recovery experiments on the synthetic mixture method and the mean percent recovery was 101.10±1.56. Repeatability and intermediate precision were rugged with %RSD values of 1.30 and 1.07, respectively. The method could separate mefenamic acid from other degradation products of forced degradation. Conclusion: The HPLC method presented herein is simple, accurate, sensitive and reproducible for the determination of mefenamic acid in an emulgel. It is served as a stability-indicating method and can be used for the analysis of the drug during product development and stability studies.

Sign in / Sign up

Export Citation Format

Share Document