Validated green chromatographic methods for determination of amlodipine and celecoxib in presence of methylacetophenone

Limit Of Detection ◽

High Sensitivity ◽

Amlodipine Besylate ◽

Rapid Methods ◽

Ich Guidelines ◽

Aim: Green, accurate and rapid methods, namely LC–MS/MS and thin layer chromatography-densitometric methods, were developed for determination of amlodipine besylate and celecoxib in presence of its process-related impurities, 4-methylacetophenone in pure and formulated tablets. Results: LC–MS/MS was achieved on ZORBAX Eclipse Plus C18 column using methanol: aqueous solution of 5 mM formic acid (95:5 v/v). High sensitivity with low limit of detection values 0.00028, 0.00027 and 0.0003 for amlodipine, celecoxib and 4-methylacetophenone, respectively were obtained. While, thin layer chromatography-densitometric was established using methanol: water: ammonia (70: 25: 1.5, by volume). Good linearity was obtained in the range of 0.1–10 μg/band, 1–150 μg/band and 0.01–2 μg/band for amlodipine, celecoxib and 4-methylacetophenone, respectively. Conclusion: The proposed method validation was achieved according to ICH guidelines. Those methods possess advantages of being ecofriendly methods which permit their application in quality control laboratories.

DETERMINATION OF 10-GINGEROL IN INDIAN GINGER BY VALIDATED HPTLC METHOD OF SAMPLES COLLECTED ACROSS SUBCONTINENT OF INDIA

International Journal of Pharmacy and Pharmaceutical Sciences ◽

10.22159/ijpps.2016v8i12.14953 ◽

2016 ◽

Vol 8 (12) ◽

pp. 190

Author(s):

Kamran Ashraf ◽

Syed Adnan Ali Shah ◽

Mohd Mujeeb

Keyword(s):

Thin Layer ◽

High Performance ◽

Limit Of Detection ◽

Limit Of Quantification ◽

Chromatography Method ◽

Aluminum Plates ◽

Layer Chromatography ◽

Hptlc Method

Objective: A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.Methods: The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F254 using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.Results: This system was found to have a compact spot of 10-gingerol at RF value of 0.57±0.03. For the proposed procedure, linearity (r2 = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.Conclusion: Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.

Rapid Thin Layer Chromatographic Determination of Aflatoxin M1 in Powdered Milk

10.1093/jaoac/68.5.952 ◽

1985 ◽

Vol 68 (5) ◽

pp. 952-954

Author(s):

Maria Luisa Serralheiro ◽

Maria Lurdes Quinta

Keyword(s):

Aqueous Solution ◽

Carbon Tetrachloride ◽

Thin Layer ◽

Limit Of Detection ◽

Chromatographic Determination ◽

Methanol Solution ◽

Aflatoxin M1 ◽

Powdered Milk ◽

Abstract A method has been developed for the detection of aflatoxin Mi in milk. The toxin is extracted with chloroform, the extract is evaporated, and the residue is partitioned between carbon tetrachloride and an aqueous saline-methanol solution. The toxin is once again extracted with chloroform from the methanol solution and analyzed by thin layer chromatography. The limit of detection of Mi in powdered milk is 0.5 μg/ kg; recoveries of added Mj are about 83%. The limit of detection can be improved to 0.3 μg/kg if the plate is sprayed with an aqueous solution of H2S04 after development.

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

Journal of AOAC International ◽

10.1093/jaoac/89.1.1 ◽

2006 ◽

Vol 89 (1) ◽

pp. 1-7 ◽

Cited By ~ 7

Author(s):

Andrés Navarrete ◽

Bharathi Avula ◽

Vaishali C Joshi ◽

Xiuhong Ji ◽

Paul Hersh ◽

...

Keyword(s):

Thin Layer ◽

High Performance ◽

Limit Of Detection ◽

Gastric Ulcers ◽

Array Detector ◽

Plant Materials ◽

Relative Standard ◽

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.

Determination of Aflatoxins, Ochratoxin A, and Zearalenone in Mixed Feeds, with Detection by Thin Layer Chromatography or High Performance Liquid Chromatography

10.1093/jaoac/64.6.1356 ◽

1981 ◽

Vol 64 (6) ◽

pp. 1356-1363 ◽

Cited By ~ 8

Author(s):

Mary V Howell ◽

Philip W Taylor

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Thin Layer ◽

High Performance ◽

Limit Of Detection ◽

Wide Range ◽

Mixed Feeds ◽

Abstract A sensitive, reliable, and economical method for the determination of 6 mycotoxins in mixed feeds is described. The feed is extracted with chloroform-water and the extract is cleaned up by using a disposable Sep-Pak silica cartridge. The procedure requires less time (15 min from sample extraction to extract preparation) and less solvent (approximately one-tenth) compared with conventional methods and is suitable for a fast, economical screen. Additional cleanup procedures, involving dialysis or extraction into base, are described for samples containing high levels of interfering compounds. Thin layer chromatography (TLC) and high performance liquid chromatography (HPLC) with fluorescence detection are described for identification and estimation of mycotoxins. The method has been applied to a wide range of mixed feeds, including laboratory animal diets, and raw materials. The limit of detection is 1 μg/kg for all mycotoxins measured by HPLC.

Determination of α-, β and γ-Amanitin by High Performance Thin-Layer Chromatography in Amanita phalloides (Vaill. ex Fr.) Seer, from Various Origin

Zeitschrift für Naturforschung C ◽

10.1515/znc-1979-1209 ◽

1979 ◽

Vol 34 (12) ◽

pp. 1133-1138 ◽

Cited By ~ 29

Author(s):

Tjakko Stijve ◽

Ruth Seeger

Keyword(s):

Thin Layer ◽

High Performance ◽

Limit Of Detection ◽

Dry Weight ◽

Amanita Phalloides ◽

Prolonged Storage ◽

Methanolic Extracts ◽

A fast, sensitive high performance thin-layer chromatographic method for the determination of α-, β-, and γ-amanitin in crude, methanolic extracts of Amanita phalloides is described. The limit of detection is 50 ng of each amanitin. With this method amanitin was determined in 24 pooled samples of Amanita phalloides, collected between 1970 and 1977 in Germany and Switzerland. The total amanitin content varied between 2010 and 7300 mg/kg dry weight and the average value was 4430 mg/kg of which 43% was α-amanitin, 49% β-amanitin and 8% γ-amanitin. The origin of the fungi hardly influenced their amanitin content: in samples collected during the same year at different sites it fluctuated within a factor of 1.7. The amanitin content of samples from the same site, but collected in different years, maximally varied within a factor of 3.7. The partial decomposition of amanitins during prolonged storage of the lyophilized samples undoubtedly contributed to this variation. Phalloidin, which was determined by conventional thin-layer-chromatography, could not be detected in a sample from 1970, whereas its concentration in material collected during 1977 amounted to 2400 mg/kg dry weight. The toxicity of the samples (LD50 of lyophilized defatted methanolic extracts intravenously for mice) varied within a factor of 2.5.

Improvement of Chemical Analysis of Antibiotics. Part XIX1: Determination of Tetracycline Antibiotics in Milk by Liquid Chromatography and Thin-Layer Chromatography/Fast Atom Bombardment Mass Spectrometry

Journal of AOAC International ◽

10.1093/jaoac/77.4.891 ◽

1994 ◽

Vol 77 (4) ◽

pp. 891-895 ◽

Cited By ~ 7

Author(s):

Hisao Oka ◽

Yoshttomo Ikai ◽

Junko Hayakawa ◽

Katsuyoshi Masuda ◽

Ken-Ichi Harada ◽

...

Keyword(s):

Thin Layer ◽

Mass Spectra ◽

High Sensitivity ◽

Tetracycline Antibiotics ◽

Coefficients Of Variation ◽

Liquid Chromatographic ◽

Layer Chromatography ◽

Fab Mass Spectra

Abstract A precise liquid chromatographic (LC) determination with high sensitivity and a reliable mass spectrometric (MS) confirmation were established for the determination of tetracycline antibiotics (TCs) in milk. The determination of the TCs was based on C18 cartridge cleanup followed by LC separation. Recoveries of TCs from milk fortified at 20 ppb were 73.0–81.8%, and coefficients of variation were 2.6–4.6%. With this method, concentrations of oxytetracycline and tetracycline as low as 10 ppb and chlortetracycline and doxycycline as low as 20 ppb were determined readily. Thin-layer chromatography (TLC)Zfast atom bombardment (FAB) MS with a condensation technique was used to confirm TCs in milk. After the C18 cartridge cleanup, separation on a C18 TLC plate, and application of the sample condensation technique, FAB mass spectra were measured. TCs in milk at 50 ppb were reliably confirmed by TLC/FABMS.

Determination of Canthaxanthin in Concentrates and Feeds

10.1093/jaoac/55.1.110 ◽

1972 ◽

Vol 55 (1) ◽

pp. 110-113

Author(s):

M Osadca ◽

M Araujo ◽

E De Ritter

Keyword(s):

Aqueous Solution ◽

Organic Solvent ◽

Thin Layer ◽

Final Solution ◽

Naturally Occurring ◽

Abstract Methods are presented for determining canthaxanthin as a 10% concentrate in beadlet form as such and in feed premixes and finished feeds. Canthaxanthin is liberated from the beadlets by hot aqueous solution and extracted into an organic solvent. In the case of feeds, separation from naturally occurring carotenoids in the extract is achieved by successive column and thin layer chromatography. Canthaxanthin in the final solution is isomerized to equilibrium with iodine and measured spectrophotometrically at 480±2 nm.

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

Journal of AOAC International ◽

10.1093/jaoac/88.5.1537 ◽

2005 ◽

Vol 88 (5) ◽

pp. 1537-1543 ◽

Cited By ~ 8

Author(s):

Caitlin Sullivan ◽

Joseph Sherma

Keyword(s):

Thin Layer ◽

Silica Gel ◽

High Performance ◽

Limit Of Detection ◽

Pharmaceutical Preparations ◽

Ultraviolet Absorption ◽

Concentration Zone ◽

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.

Colorimetric Determination of Terreic Acid Produced by Aspergillus terreus

10.1093/jaoac/61.3.581 ◽

1978 ◽

Vol 61 (3) ◽

pp. 581-583

Author(s):

Thirugnana Subramanian ◽

Kuppuswamy Mohan Namasivayam ◽

Edayathimangalam R B Shanmugasundaram

Keyword(s):

Thin Layer ◽

Ethyl Acetate ◽

Lower Limit ◽

Minimal Medium ◽

Aspergillus Terreus ◽

Limit Of Detection ◽

Colorimetric Determination ◽

Abstract Two methods have been developed for determining terreic acid, which is a mycotoxin produced by Aspergillus terreus, a common food contaminant. The organism was grown independently in synthetic minimal medium, bread, and rice. After 15 days of growth, the toxin was extracted with ethyl acetate, cleaned up by thin layer chromatography, and determined colorimetrically, using Folin's reagent or 2,4- dinitrophenylhydrazine. The production of terreic acid was greater on bread than on rice or minimal medium. Recoveries of 200–400 ≧g terreic acid/100 g bread and rice ranged from 62 to 98%. The lower limit of detection was 200 ≧g/100 g.

Validation of Thin-Layer Chromatography-Bioautographic Method for Determination of Streptomycin

JURNAL FARMASI DAN ILMU KEFARMASIAN INDONESIA ◽

10.20473/jfiki.v4i12017.34-38 ◽

2018 ◽

Vol 4 (1) ◽

pp. 34

Author(s):

Isnaeni Isnaeni ◽

Andri Astuti ◽

Muhammad Yuwono

Keyword(s):

Thin Layer ◽

Limit Of Detection ◽

System Optimization ◽

Detection Accuracy ◽

Nutrient Agar Medium ◽

Bioautographic Method ◽

Layer Chromatography ◽

Bio Assay

Background: A simple bio-assay for determination of streptomycin hyphenated with planar chromatography techniques was developed. Objective: This study aims to validate the method for identification and determination of streptomycin in injection preparations with TLC-bioautography. Methods: Thin Layer Chromatography (TLC) was performed on the silica Gel GF-254 using KH2PO4 solution as mobile solvent. The visualization was performed by spraying 2% resorcinol. Direct bi autography was developed using Escherichia coli ATCC 25922 as a bacterial test, grown on the nutrient agar medium at 37oC for 24 hours. The method was validated corresponding to linearity, limit of detection (LOD), intra day precision, and accuracy parameters. The accuracy was measured using streptomycin injection as a sample. Results: The Results showed that the KH2PO4 solution at 7.5% concentration was found to be the optimized solvent with Rf value of 0.5. The linear equation was y = 10.176x + 4.046 at 150 - 350 µg/mL concentration range with the linearity coefficient, Limit of Detection, accuracy, and variation coefficient were 0.9907; 40 ppm; 96.37 + 2.22% (with an RSD value of 2.31%); and 1.63 respectively. Conclusion: The prospective TLC-bioautographic method was applied for the identification and determination of streptomycin in a preparation using a single eluent KH2PO4. The eluent system optimization remains necessary for the identification and determination of the mixture of streptomycin with other antibiotics, such as aminoglycoside groups.