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 ◽  
...  

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.

Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb

<p><strong>Objective: </strong>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.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 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.</p><p><strong>Conclusion: </strong>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.</p>


2020 ◽  
Vol 412 (27) ◽  
pp. 7441-7451
Author(s):  
Claudia Oellig ◽  
Max Blankart ◽  
Jörg Hinrichs ◽  
Wolfgang Schwack ◽  
Michael Granvogl

Abstract Mono- and diacylglycerol (MAG and DAG) emulsifiers (E 471) are widely applied to regulate techno-functional properties in different food categories, for example, in dairy products. A method for the determination of MAG and DAG in aerosol whipping cream by high-performance thin-layer chromatography with fluorescence detection (HPTLC–FLD) after derivatization with primuline was developed. For sample preparation, aerosol whipping cream was mixed with ethanol, followed by the addition of water and liquid-liquid extraction with tert-butyl methyl ether. The sample extracts were analyzed by HPTLC–FLD on silica gel LiChrospher plates with n-pentane/n-hexane/diethyl ether (22.5:22.5:55, v/v/v) as mobile phase, when interfering matrix like cholesterol and triacylglycerols were successfully separated from the E 471 food additives. For quantitation, an emulsifier with known composition was used as calibration standard and the fluorescent MAG and DAG were scanned at 366/> 400 nm. Limits of detection and quantitation of 4 and 11 mg/100 g aerosol whipping cream were obtained for both monostearin and 1,2-distearin, respectively, and allowed the reliable quantitation of MAG and DAG from E 471 far below commonly applied emulsifier amounts. Recoveries from model aerosol whipping cream with 400 mg E 471/100 g were determined in a calibration range of 200–600 mg E 471/100 g sample and ranged between 86 and 105% with relative standard deviations below 7%. In aerosol whipping creams from the German market, E 471 amounts ranged between 384 and 610 mg/100 g.


1981 ◽  
Vol 64 (6) ◽  
pp. 1356-1363 ◽  
Author(s):  
Mary V Howell ◽  
Philip W Taylor

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.


1979 ◽  
Vol 34 (12) ◽  
pp. 1133-1138 ◽  
Author(s):  
Tjakko Stijve ◽  
Ruth Seeger

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.


2005 ◽  
Vol 88 (5) ◽  
pp. 1537-1543 ◽  
Author(s):  
Caitlin Sullivan ◽  
Joseph Sherma

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.


2008 ◽  
Vol 91 (5) ◽  
pp. 1203-1209 ◽  
Author(s):  
Tomasz Tuzimski

Abstract High-performance thin-layer chromatography with diode array scanning (TLC-DAD) and high-performance column liquid chromatography with a diode array detector (HPLC-DAD) were used to screen water samples for pesticides. Atrazine, clofentezine, chlorfenvinphos, hexaflumuron, terbuthylazine, lenacyl, neburon, bitertanol, and metamitron were enriched from canal water samples by solid-phase extraction (SPE) on octadecyl silane (C18)/styrene-divinylbenzene-1, C18, C18 Polar Plus, and cyanopropyl (CN) cartridges. Recovery rates were high for all extraction materials except CN, for which values for all pesticides were lower. SPE was used for both preconcentration and fractionation of the analytes. Analytes were eluted by means of methanol and dichloromethane. Methanol eluates were analyzed by HPLC-DAD and dichloromethane eluates by TLC-DAD. The method was validated for precision, repeatability, and accuracy. Calibration graphs were linear between 0.1 and 50.0 g/mL for all pesticides, and correlation coefficient (r) values were between 0.9994 and 1.000 as determined by HPLC-DAD. Calibration graphs were linear between 0.1 and 1.5 g/spot for all pesticides, and r values were between 0.9899 and 0.9987 as determined by TLC-DAD. The limit of detection was between 0.04 and 0.23 g/spot for TLC-DAD and 0.02 and 0.45 g/mL for HPLC-DAD.


2008 ◽  
Vol 91 (5) ◽  
pp. 1186-1190 ◽  
Author(s):  
Urszula Hubicka ◽  
Jan Krzek ◽  
Justyna uka

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.


2020 ◽  
pp. 215-222
Author(s):  
Ol'ga Valer'yevna Trineeva ◽  
Aleksey Ivanovich Slivkin

An analysis of the literature over the past 20 years has shown that when controlling the quality of drugs containing monosaccharides, as well as studying the composition of simple sugars in polysaccharide complexes of medicinal plants and not only, preference is given to physicochemical methods, as the most express, sensitive and informative. No means have been found in the scientific literature to identify and quantify simultaneously various monosaccharides by high performance thin layer chromatography (HPTLC). An economical and rapid method has been developed for the identification and quantitative determination of simple reducing sugars (by the example of glucose, rhamnose and xylose) by the HPTLC method. The optimal conditions for their chromatography in a thin layer of sorbent with a quantitative interpretation of HPTLC data on a personal computer were experimentally selected and theoretically substantiated. In a detailed study of the influence of the polarity of the system on the value of Rf, the intervals of values of the polarity of the eluent were chosen, in which these dependences become linear. Using the proposed dependencies, you can select different systems for the separation of monosaccharides in a thin layer of sorbent, so that the value of Rf fit into the optimal values. The proposed method was tested on medicinal plant raw materials of nettle dioica and sea buckthorn fruits of various conservation methods. Zones of simple sugars of characteristic color were found on the chromatograms of extracts from the studied raw materials, among which glucose, xylose and rhamnose were identified by the characteristic value of Rf values in comparison with reliable standard samples. The technique can be used in quality control of substances, single-component and complex preparations, plant objects, dietary supplements, premixes and products of the food industry.


2006 ◽  
Vol 89 (4) ◽  
pp. 995-998 ◽  
Author(s):  
Magdalena Wójciak-Kosior ◽  
Agnieszka Skalska ◽  
Grażyna Matysik ◽  
Magdalena Kryska

Abstract In this paper, a high-performance thin-layer chromatography (HPTLC) method combined with densitometry has been described. Chromatography was performed on silica gel Si 60F254 plates using dichloromethaneethyl acetateformic acid (9.5 + 0.5 + 0.1, v/v) mobile phase. This method has been successfully applied for the determination of phenobarbital in pharmaceuticals. Obtained results were comparable with traditionally used column high-performance liquid chromatography (HPLC) methods. For the proposed procedure, linearity (r &gt; 0.999), sensitivity (limit of detection 0.4 g/spot), recovery (97.8102.1%), and repeatability were found to be satisfactory. The HPTLC-densitometry method has many advantages, such as simplicity, reasonable sensitivity, rapidity, and low cost, and it can be successfully used in routine quality control of multidrug preparations containing barbiturates.


2005 ◽  
Vol 88 (5) ◽  
pp. 1525-1529 ◽  
Author(s):  
Dorota Kowalczuk

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].


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