scholarly journals High-Performance Thin-Layer Chromatography with Densitometry for the Determination of Ciprofloxacin and Impurities in Drugs

2005 ◽  
Vol 88 (5) ◽  
pp. 1530-1536 ◽  
Author(s):  
Jan Krzek ◽  
Urszula Hubicka ◽  
Justyna Szczepańczyk
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
High Sensitivity ◽  
Good Precision ◽  
Relative Standard ◽  
Tlc Plates ◽  
Quantitative Analyses

Abstract A thin-layer chromatographic (TLC)-densitometric method has been developed for identification and quantification of ciprofloxacin (Rf = 0.61) and an ethylenediamine compound (Rf = 0.42), a desfluoro compound (Rf = 0.48), by-compound A (Rf = 0.53), and fluoroquinolonic acid (Rf = 0.68) as ciprofloxacin degradation products in pharmaceutical preparations. By using chloroform–methanol–25% ammonia (43 + 43 + 14, v/v/v) as the mobile phase and silica gel 60 F254 high-performance TLC plates as the stationary phase, it was possible to separate individual constituents that, when subjected to ultraviolet (UV) densitometric analysis at 330 nm for fluoroquinolonic acid and 277 nm for the other compounds, gave well developed peaks allowing easy qualitative and quantitative analyses. DMSO–methanol (1 + 1) was used to extract drug constituents. The method showed high sensitivity (limit of detection 10 to 44 ng), a wide linearity range (3 to 20 μg/mL), and good precision (2.32 to 6.46% relative standard deviation) and accuracy (percentage recoveries 98.62 to 101.52%) for individual constituents.

scholarly journals Densitometric High Performance Thin-Layer Chromatography Identification and Quantitative Analysis of Psychotropic Drugs

2005 ◽  
Vol 88 (1) ◽  
pp. 70-79 ◽  
Author(s):  
Anna Maślanka ◽  
Jan Krzek
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Psychotropic Drugs ◽  
High Performance ◽  
Limit Of Detection ◽  
High Sensitivity ◽  
Experimental Conditions ◽  
Mobile Phases ◽  
Tlc Plates ◽  
Layer Chromatography

Abstract A thin-layer chromatography (TLC)-densitometry method has been developed to identify and quantify haloperidol, amitriptyline, sulpiride, promazine, fluphenazine, doxepin, diazepam, trifluoperazine, clonazepam, and chlorpromazine in selected psychotropic drugs. Separation was performed on precoated silica gel 60 F254 TLC plates. Chromatograms were developed in various mobile phases, and 8 of 30 tested phases were selected based on spot location and developing time. The identification and quantification were carried out based on ultraviolet densitometric measurements at chosen wavelengths. In addition to retention coefficients, the absorption spectra recorded directly from chromatograms were also used in qualitative analysis. Under established experimental conditions, high sensitivity of the method was achieved. The limit of detection ranged from 0.009 to 0.260 μg, depending on the wavelength selected for measuring. A satisfactory recovery, ranging from 92.99 to 104.70%, was achieved for individual constituents.

scholarly journals Quantitative Determination of Triterpenes from Amphiptherygium adstringens by Liquid Chromatography and Thin-Layer Chromatography and Morphological Analysis of Cuachalalate Preparations

2006 ◽  
Vol 89 (1) ◽  
pp. 1-7 ◽  
Author(s):  
Andrés Navarrete ◽  
Bharathi Avula ◽  
Vaishali C Joshi ◽  
Xiuhong Ji ◽  
Paul Hersh ◽  
...  
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Gastric Ulcers ◽  
Array Detector ◽  
Plant Materials ◽  
Relative Standard ◽  
Layer Chromatography

Abstract Amphiptherygium adstringens (Anacardiaceae/Julianaceae), local name cuachalalate, is used in folk medicine for the treatment of cholelithiasis, fevers, fresh wounds, hypercholesterolemia, gastritis, gastric ulcers, and cancer of the gastrointestinal tract. The development of column high-performance liquid chromatographyphotodiode array detector (LC-PDA) and high-performance thin-layer chromatography (HPTLC)densitometry methods for the determination of masticadienonic acid and 3-hydroxymasticadienonic acid in cuachalalate preparations is described in this paper. Good separation of the compounds could be achieved by both methods. Either might be preparable depending on the requirements. The LC separation was performed on a Phenomenex Synergi MAX-RP 80A reversed-phase column operated at 40C with detection at 215 nm. The plant materials were extracted with methanol by sonication. The triterpenes present in the plant material and commercial extracts were separated with an acetonitrilewater reagent alcohol isocratic system. The limit of detection was 0.10.2 g/mL. The relative standard deviation values for the determination of triterpenes in plant extracts were less than 1.00%. This is the first report of an analytical method developed for the quantitative analysis of triterpenes from Amphiptherygium adstringens by LC-PDA and HPTLC. The stem bark showed higher amounts of triterpenes, and low amounts in root and stem root. The microscopic description of the crude drug of cuachalalate was also provided.

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 and Validation of a Method for Determination of Caffeine in Diuretic Tablets and Capsules by High-Performance Thin-Layer Chromatography on Silica Gel Plates with a Concentration Zone Using Manual Spotting and Ultraviolet Absorption Densitometry

2005 ◽  
Vol 88 (5) ◽  
pp. 1537-1543 ◽  
Author(s):  
Caitlin Sullivan ◽  
Joseph Sherma
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Silica Gel ◽  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Ultraviolet Absorption ◽  
Concentration Zone ◽  
Layer Chromatography

Abstract A new quantitative method using silica gel high-performance thin-layer chromatography plates with channels and a concentration zone, manual application of standards and samples, development with methanol–ethyl acetate (15 + 85) mobile phase, and ultraviolet absorption densitometry is reported for the determination of caffeine in diuretic pharmaceutical preparations. Tablet and capsule products containing potassium salicylate, acetaminophen, and salicylamide as active ingredients were analyzed to test the applicability of the new method, and precision, accuracy, linearity, limits of detection and quantitation, and selectivity were validated. The milligrams of caffeine in each tablet ranged from 48.0 to 51.0, and the milligrams in each capsule from 37.9 to 40.3. Within-day precision was 1.48 and 1.78% (n = 6), and interday precision 0.723 and 1.26% (n = 5) for analysis of 2 tablets and 2 capsules, respectively. Accuracy validation of the tablet and capsule results produced errors of 1.0 and 1.9% for spiked blank analyses and 2.6 and 3.5% for standard addition analyses, respectively. A comparative study using a caffeine standard solution and a multicomponent analgesic tablet solution containing caffeine, acetaminophen, and acetylsalicylic acid showed that manual application on the concentration zone, instrumental application on the concentration zone, and instrumental application on the silica gel gave quite similar results in terms of number of theoretical plates, resolution, limit of detection, and linearity.

scholarly journals Thin-Layer Chromatography-Densitometric Measurements for Determination of N-(Hydroxymethyl)nicotinamide in Tablets and Stability Evaluation in Solutions

2008 ◽  
Vol 91 (5) ◽  
pp. 1186-1190 ◽  
Author(s):  
Urszula Hubicka ◽  
Jan Krzek ◽  
Justyna uka
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Limit Of Detection ◽  
Good Precision ◽  
First Order ◽  
Kinetic And Thermodynamic Parameters ◽  
Relative Standard ◽  
Basic Solutions ◽  
Layer Chromatography

Abstract A thin-layer chromatography (TLC)-densitometric method was developed to determine N-(hydroxymethyl)nicotinamide in tablets and basic solutions along with nicotinic acid. Analysis was performed on silica gel F254 plates using chloroformethanol (2 + 3, v/v) mobile phase. The densitometric observations were made at 260 nm. The results showed good precision and accuracy; relative standard deviation was 2.37, and recovery ranged from 97.60 to 100.82. The limit of detection was 0.1 g/spot, while the linearity range was from 0.2 to 1.75 g/spot. Applicability of the newly developed method was tested for determination of N-(hydroxymethyl)nicotinamide in the preparation Cholamid&lt;sup/&gt;. Densitometric measurements were used to evaluate stability of N-(hydroxymethyl)nicotinamide in basic solutions. It was found that decomposition corresponded to first-order reaction kinetics. The computed kinetic and thermodynamic parameters at 30C were as follows: k 0.00675/min, t0,5 1.71 h, t0,1 0.26 h, and Ea 44.75 kJ/mol.

Fluoroimmunoassay Based on FITC-Labeled Antibody for the Determination of Estradiol

2014 ◽  
Vol 960-961 ◽  
pp. 3-6
Author(s):  
Long Jun Wang ◽  
Wei Li Xue ◽  
Ling Yun Du
Keyword(s):  
Human Urine ◽  
High Performance ◽  
Solid Phase ◽  
High Sensitivity ◽  
Good Precision ◽  
Experimental Conditions ◽  
Time Saving ◽  
Relevant Variable ◽  
Relative Standard

A new fluorescence immunoassay with high sensitivity, time-saving, good precision and reliablility was proposed for the determination of estradiol (E2) in human urine. The complex of FITC-labeled anti-E2antibody was produced and regarded as a probe in this system. Ninety-six microplate was coated with ovalbumin conjugated E2antigen as solid phase for the immunoassay. The method parameters affecting the determination, such as the concentration of immunoreagents, pH, and other relevant variable conditions upon the immunoassay were studied and optimized systematically. Under the optimal experimental conditions, it was found that the proposed method exhibited high performance with the detection limit of 9.2 pg/mL, and the linear range of determination of 0.01-1000 ng/mL. The recoveries were 93.58-105.82% with the relative standard deviations (RSD) 5.52-7.09%. The proposed method has been used for the determination of E2in human urine with satisfactory results, and may be expected to find wide application in other environmental samples.

scholarly journals HPLC–DAD method for investigating pantoprazole for its stress-dependent degradation by photolysis and oxidation

2020 ◽  
Vol 32 (4) ◽  
pp. 247-255
Author(s):  
Mohammad Al Bratty ◽  
Neelaveni Thangavel ◽  
Ramalingam Peraman ◽  
Vinod Kumar ◽  
Padmanabha Reddy ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Stress Conditions ◽  
Linear Regression Coefficient ◽  
Intermediate Precision ◽  
Photolytic Degradation ◽  
Relative Standard ◽  
Array Detection ◽  
Stress Dependent

A reversed-phased high-performance liquid chromatography–diode-array detection (HPLC–DAD) method has been developed for investigating the stress-dependent degradation of pantoprazole (PTZ) by a photolytic and oxidative mechanism. The developed method separated PTZ from its degradation products on a C18 column with a mobile phase consisted of methanol and water (60:40, v/v; pH 3.0) at a flow rate of 1 mL/min. The linear regression coefficient of 0.9995 was obtained for a concentration range from 5 to 25 μg/mL. The % relative standard deviation for repeatability and intermediate precision were below 0.5% and 1.5%, respectively, while the sensitivity of the method was demonstrated by a limit of detection value of 0.25 μg/mL. The stress sample analyses for PTZ results revealed the formation of a total of 18 degradation products, and out of them, 9 degradation products were common for both photolytic and oxidative degradations. Further, the oxidation by azobisisobutyronitrile produced the highest number of degradation products (11 impurities), 3 of which are more hydrophobic than PTZ. In photolytic degradation, 8 and 7 degradation products were observed with UV radiation and sunlight exposure, respectively. Furthermore, the degradation of pantoprazole sodium injection formulation was carried out under the same stress conditions, and it revealed the formation of 3 common impurities under both stress conditions, but other impurities were not detected in the formulations. Finally, 3 common impurities formed in formulations of PTZ injections, viz., sulfone, N-oxide, and N-oxide sulfone impurities, were identified by spike analyses.

scholarly journals Simultaneous High-Performance Thin-Layer Chromatography Densitometric Assay of Trandolapril and Verapamil in the Combination Preparation

2005 ◽  
Vol 88 (5) ◽  
pp. 1525-1529 ◽  
Author(s):  
Dorota Kowalczuk
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Ethanol Acetic Acid ◽  
Relative Standard ◽  
Satisfactory Precision ◽  
Tlc Plates ◽  
Combination Preparation ◽  
Layer Chromatography

Abstract A high-performance thin-layer chromatography (TLC) method coupled with densitometric analysis has been developed for simultaneous measurement of trandolapril (TRA) and verapamil (VER) in 2-component mixtures and in their combination capsules. The active substances were extracted from capsules withmethanol (mean recovery: 103.4% for TRA, 97.13% for VER) and chromatographed on TLC plates coated with silica gel 60 F254 in horizontal chambers with ethyl acetate–ethanol–acetic acid (8 + 2 + 0.5, v/v) mobile phase. Chromatographic separation of these components was followed by ultraviolet densitometric quantification at 215 nm. The calibration graphs were constructed over the concentration range from 0.5 to 1.5 μg/μL (corresponding to 5.0–15.0 μg/spot for both drugswith good correlation (r ≥ 990). Detection and quantitation limits were found to be 1.25 and 3.75 μg/spot for TRA and 0.15 and 0.45 μg/spot for VER, respectively. The proposed method was used for determination of both drugs in TRA-VER capsules with satisfactory precision [0.97% &lt; relative standard deviation (RSD) &lt;4.50% for TRA, 0.49% &lt; RSD &lt; 3.10% for VER] and accuracy [2.16% &lt; relative error (RE) &lt; 4.90% for TRA, 1.73% &lt; RE &lt; 5.68% for VER].

Recent Applications of High Performance Thin Layer Chromatography and Derivative Spectrophotometry in Pharmaceutical Analysis

2020 ◽  
Vol 16 (6) ◽  
pp. 671-689
Author(s):  
Marcin Gackowski ◽  
Marcin Koba ◽  
Katarzyna Mądra-Gackowska ◽  
Piotr Kośliński ◽  
Stefan Kruszewski
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Pharmaceutical Analysis ◽  
High Performance ◽  
Degradation Products ◽  
Derivative Spectrophotometry ◽  
Accuracy And Precision ◽  
Post Marketing ◽  
Layer Chromatography

At present, no one can imagine drug development, marketing and post-marketing without rigorous quality control at each stage. Only modern, selective, accurate and precise analytical methods for determination of active compounds, their degradation products and stability studies are able to assure the appropriate amount and purity of drugs administered every day to millions of patients all over the world. For routine control of drugs simple, economic, rapid and reliable methods are desirable. The major focus of current scrutiny is placed on high-performance thin layer chromatography and derivative spectrophotometry methods, which fulfill routine drug estimation’s expectations [1-4]. The present paper reveals state-of-the-art and possible applications of those methods in pharmaceutical analysis between 2010 and 2018. The review shows advantages of high-performance thin layer chromatography and derivative spectrophotometry, including accuracy and precision comparable to more expensive and time-consuming methods as well as additional fields of possible applications, which contribute to resolving many analytical problems in everyday laboratory practice.

ICH/FDA Guidelines-Compliant Validated Stability-Indicating HPLC-UV Method for the Determination of Axitinib in Bulk and Dosage Forms

2020 ◽  
Vol 16 (8) ◽  
pp. 1106-1112
Author(s):  
Ibrahim A. Darwish ◽  
Nasr Y. Khalil ◽  
Mohammad AlZeer
Keyword(s):  
High Performance ◽  
Kinase Inhibitor ◽  
Degradation Products ◽  
Internal Standard ◽  
Dosage Forms ◽  
Uv Detector ◽  
Stability Indicating ◽  
Therapeutic Benefits ◽  
Relative Standard

Background: Axitinib (AXT) is a member of the new generation of the kinase inhibitor indicated for the treatment of advanced renal cell carcinoma. Its therapeutic benefits depend on assuring the good-quality of its dosage forms in terms of content and stability of the pharmaceutically active ingredient. Objective: This study was devoted to the development of a simple, sensitive and accurate stabilityindicating high-performance liquid chromatographic method with ultraviolet detection (HPLC-UV) for the determination of AXT in its bulk and dosage forms. Methods: Waters HPLC system was used. The chromatographic separation of AXT, internal standard (olaparib), and degradation products were performed on the Nucleosil CN column (250 × 4.6 mm, 5 μm). The mobile phase consisted of water:acetonitrile:methanol (40:40:20, v/v/v) with a flow rate of 1 ml/min, and the UV detector was set at 225 nm. AXT was subjected to different accelerated stress conditions and the degradation products, when any, were completely resolved from the intact AXT. Results: The method was linear (r = 0.9998) in the concentration range of 5-50 μg/ml. The limits of detection and quantitation were 0.85 and 2.57 μg/ml, respectively. The accuracy of the method, measured as recovery, was in the range of 98.0-103.6% with relative standard deviations in the range of 0.06-3.43%. The results of stability testing revealed that AXT was mostly stable in neutral and oxidative conditions; however, it was unstable in alkaline and acidic conditions. The kinetics of degradation were studied, and the kinetic rate constants were determined. The proposed method was successfully applied for the determination of AXT in bulk drug and dosage forms. Conclusions: A stability-indicating HPLC-UV method was developed and validated for assessing AXT stability in its bulk and dosage forms. The method met the regulatory requirements of the International Conference on Harmonization (ICH) and the Food and Drug Administration (FDA). The results demonstrated that the method would have great value when applied in quality control and stability studies for AXT.

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