Direct Fluorescent Detection of Organothiophosphorus Pesticides and Some of Their Sulfur-containing Breakdown Products After Thin Layer Chromatography

1967 ◽  
Vol 50 (5) ◽  
pp. 1088-1098
Author(s):  
Mohamed Tawfik H Ragab

Abstract A rapid, simple, convenient, and widely applicable method for the direct fluorescent detection of organothiophosphorus pesticides and some postulated breakdown products of these compounds is presented. The coinpounds were spotted on thin layer chromatographic sheets, developed in ethyl acetate :nhexane, and made visible by exposure to bromine vapor followed by spraying with ferric chloride and 2-(o-hydroxy phenyl) benzoxazole. Of the 47 compounds tested, 32 compounds produced fluorescent blue spots vinder longwave ultraviolet light; these consisted of 25 organothiophosphorus pesticides, 5 sulfur-containing breakdown products, and phosphoric and hypophosphorous acids. A superimposed Congo red spray destroyed the fluorescence and resulted in dark blue spots against a red backgrovind. The sensitivity of this method is in the range of 0.2 to 5.0 μg, depending on the specific compound.

Author(s):  
Dharmendra B. Sharma ◽  
Parth Aphale ◽  
Vineet Sinnarkar ◽  
Sohan S. Chitlange ◽  
Asha Thomas

Background: Chromatography is one of the important laboratory technique in which the components of a mixture are separated on an adsorbent in order to analyze, identify, purify and quantify a mixture. Thin Layer Chromatography (TLC)is used to support the identity of a compound in a mixture when the Rf of a compound is compared with the Rf of a known compound. High Performance Thin Layer Chromatography is a sophisticated and automated form of Thin Layer Chromatography (TLC). The procedure simultaneously processes the sample and standard that results in better analytical precision and accuracy at a faster pace. Pharmacological/ Toxicological action of Nux Vomica is because of its active principles present in the seeds namely strychnine, brucine etc. This research paper aims to corelate the active principles present in Nux Vomica with the toxicological action of the same. Materials and Methods: 1. Standard Nux Vomica mother tincture was tested for its alkaloid markers and its correlation with the toxicological action was studied. 2. Analysis of the mother tincture was done using High Performance Thin Layer Chromatography. 3. Stationary phase consisted of TLC Aluminium sheets with silica gel 60 F253 pre-coated layer (20cm x 10cm), thickness-0.2mm, no. of tracks-18, band length-6mm. 4. Mobile Phase consisted of Chloroform: Methanol (9.5:0.5). 5. The plate was developed in developing chamber and observed under U.V. Light. Results: Colours seen on the HPTLC Plates of samples are greenwhich corresponds to strychnine, dark blue which corresponds to brucine, orange to alkaloids fluorescent green to sterols and pink to fatty acids which are evident on the chromatogram. Conclusion: Therapeutic action of Nux Vomica as noted in Homoeopathic Materia Medica is because of the active principles like strychnine, brucine, alkaloids, sterols, fatty acids present in it which is evident from the chromatogram.


Author(s):  
Neelutpal Gogoi ◽  
Biman Bhuyan ◽  
Trinayan Deka

Objectives: In this study, systematic pharmacognostic study and preliminary phytochemical screening of the bark of Cascabela thevetia L. were carried out. Methods: The selected plant part was collected, processed and stored in an airtight container. From the bark different pharmacognostic studies like macroscopic and microscopic evaluation, physicochemical parameters, fluorescence analysis were done. Powdered bark was successively extracted by petroleum ether, chloroform, ethyl acetate, and methanol using a Soxhlet apparatus and finally macerated with the hydro-alcoholic solvent system (30:70). The preliminary phytochemical analysis and thin layer chromatography of the extracts were done to find the nature and number of the different phytoconstituents present. Results: Transverse microscopy reveals the presence of crystal oxalate, cork cell, starch granules, vascular bundle, phloem fiber, parenchyma cells, and collenchyma cells. Powder microscopy also showed the presence of cork cell, fiber and calcium oxalate crystal. Results obtained in different physicochemical analysis like total ash, acid insoluble ash, water soluble ash, alcohol-soluble extractive, water-soluble extractive, and moisture content were 8.67%, 0.83%, 5.33%, 4.53%, 12.27%, and 7.83% respectively. Phytochemical analysis showed the presence of alkaloid, flavonoid, triterpenoid, phytosterol, tannin, saponin, anthraquinone, carbohydrate and fatty acid in the different extracts. TLC (Thin Layer Chromatography) study revealed 4 spots in petroleum ether, chloroform, ethyl acetate, and methanol extracts and 3 spots in the Hydro-alcoholic extract with different solvent systems. Conclusion: The results obtained from the study will provide a reliable basis for identification, purity, and quality of the plant.


1975 ◽  
Vol 21 (1) ◽  
pp. 76-80 ◽  
Author(s):  
H Kenneth Sleeman ◽  
James A Cella ◽  
Johnnie L Harvey ◽  
Douglas J Beach

Abstract A procedure for detecting methaqualone and identifying methaqualone metabolites in urine by thin-layer chromatography is described and evaluated. Urine is hydrolyzed with HCl or NalO4, adjusted to pH 9.5, and extracted with chloroform. The chloroform extract is evaporated, reconstituted in methanol, applied to fluorescent silica-gel plates, and developed with ethyl acetate:methanol:ammonium hydroxide (28%) (85:10:5 by vol). Methaqualone use is detected by a pattern of four metabolites, which can be seen under ultraviolet light or are made visible by acidified iodoplatinate reagent. Synthetic methaqualone metabolites are used for identification and to compensate for procedural variables. More than 250 positive urine specimens were correctly identified by this method. Hydrolyzed natural and synthetic metabolites were identical by several criteria.


1974 ◽  
Vol 57 (5) ◽  
pp. 1026-1032
Author(s):  
Raja J Ismail ◽  
Frances L Bonner

Abstract Reverse phase partition thin layer chromatography is described for the separation of the different components in polychlorinated biphenyl compounds, chlordane, and toxaphene. Plates prepared from washed aluminum oxide, with silver nitrate incorporated into the layer, are saturated with a nonpolar solvent (immobile phase), air-dried overnight, and spotted. A mixture of polar solvents is used as the mobile phase. After exposure to longwave ultraviolet light, dark blue silver chloride spots form on a white background. As little as 1 μg Aroclor can be detected by this method, which can be applied for qualitative and semiquantitative measurements. Distinct patterns are obtained for Aroclor reference materials which are resolved from most DDT analogs and other commonly occurring chlorinated pesticides. Since the use of infrared, ultraviolet, nuclear magnetic resonance, and mass spectroscopy as supplementary methods for qualitative analysis involves a large capital outlay which is often beyond the resources of small laboratories, the technique is most valuable to the chemist in such laboratories where time and money are important factors.


Author(s):  
Mustafa H. Alwan ◽  
Maha N. Hamad

  Convolvulus arvensis is a species of bindweed that is rhizomatous and is in the morning glory family (Convolvulaceae) native to Europe and Asia. The plant is naturally grown in Iraq. The plant was reported to be used in traditional medicine from as early as 1730s. The Aerial parts of Convolvulus arvensis were macerated in 80% ethanol for 6 days. The concentrated extract was partitioned with n-hexane, chloroform, ethyl acetate- and n-butanol successively. The n-hexane and ethyl acetate, fractions were examined for the presence of phytochemicals by thin layer chromatography and high performance liquid chromatography and its steroid and flavonoid contents were investigated. Stigmasterol was isolated from n-hexane fraction and identified by liquid chromatography/mass spectroscopy. Rutin was isolated from the ethyl acetate fraction and identified by liquid chromatography/mass spectroscopy. The aim is to examine the phytochemical constituents of the aerial parts of Convolvulus arvensis, literature survey available so far revealed that there were no studies about the phytochemical investigation for Convolvulus arvensis in Iraq.  Different chromatographic techniques like Thin Layer Chromatography and mass spectroscopy were used and the presence of Stigmasterol and Rutin in aerial parts of Convolvulus arvensis was indicated.  


2019 ◽  
Vol 1 (1) ◽  
pp. 1-6
Author(s):  
Aji Suteja ◽  
Emmy Harso Kardhinata ◽  
Rosliana Lubis

This study aims to determine how to identify the types of secondary metabolite compounds contained in durian leaves. The study was conducted by an experimental method by identifying secondary metabolite compounds on durian leaves using phytochemical screening. The sample criteria used were the leaf buds and all the leaf strands (except the leaf bones). The results of the study showed that of the three types of durian leaves namely copper, baskets and Sp A. There are several types of secondary metabolite compounds including alkaloids, steroids, and terpenoids. Phytochemical screening analysis was carried out using thin layer chromatography by showing RF values on three types of durian leaves using methanol and ethyl acetate solvents in a ratio of 3: 1. RF value on copper durian is 0.97, bakul durian is 0.95 and Sp durian. A 0.94.


ALCHEMY ◽  
2013 ◽  
Author(s):  
Noer Mardlatillah Sharo ◽  
Rachmawati Ningsih ◽  
Ahmad Hanapi ◽  
Ahmad Nasichuddin

<p><em>Eucheuma cottonii</em> is a multicellular algae (multicellular) that have bioactive compounds used in medicine, such as anticancer. The purpose of this research is to know the level of toxicity of the crude extract of ethanol and n-hexane red algae (<em>Eucheuma cottonii</em>) against larvae of shrimp <em>A</em><em>. salina</em> Leach and to know the active compounds contained in crude extracts of ethanol and n-hexane red algae (<em>Eucheuma cottonii</em>).</p><p>This research was conducted with the maceration extraction continuing by test toxicity against the shrimp larvae of <em>A</em><em>. salina</em> Leach (BSLT). The result of the toxicity test then proceeds with the test reagents and phytochemicals with thin layer chromatography for positive test of compound phytochemicals. Thin-layer chromatography using eluen n-hexane: ethyl acetate (7: 3) to ethanol extract and n-hexane: ethyl acetate (17: 3) for n-hexane extract. Data on toxicity of <em>A. salina Leach</em><em> </em>analyzed by probit analysis to find out the value of LC<sub>50</sub> on each extract.</p><p>The results of this research indicate that each of the rough red algae extract (<em>Eucheuma cottonii</em>) by using a solvent of ethanol and n-hexane have toxicity values (LC<sub>50</sub>) of shrimp larvae of <em>A</em><em>. salina</em> Leach consecutive 58,0128 ppm and 61,7571 ppm. Active compounds content of Phytochemical test results i.e. triterpenoid (ethanol extract) and steroids (n-hexsane extract). The TLC triterpenoid obtained 7 stains, and the results obtained steroids 8 TLC stains.</p>


ALCHEMY ◽  
2013 ◽  
Author(s):  
Roihatul Muti'ah ◽  
Elok Kamilah Hayati ◽  
Yani Triastutik

<p>The purpose of this research wasto separate and identify the leaf crude extracts esquiterpene of Sun flower (<em>Helianthus annuus</em> L.) using thin layer chromatography.<strong></strong></p><p>Sun flower leaf maceration method performed with the solvent methanol. Then performed liquid extraction with ethyl acetate and n-hexane solvent. Ethyl acetate extract fraction and n-hexane extract fraction furth erphyto chemical test. After being test edphyto chemical with reagents, both extracts was followed by sesquiterpene content identification using thin layer chromatography (TLC)  analytic.<strong></strong></p>Phytochemical test result from ethyl acetate extract fraction was positive terpenoid, sesquiterpene and triterpene, while n-hexane extractfraction positive terpenoid, sesquiterpene andsteroid. All egedsesquiterpene with eluentdichloromethane: ethyl acetate (4,8:0,2) is shown with apurplestain. In the ethyl acetate extract fraction all egedsesquiterpene having Rf values of 0.89; 0.94, and 0.96. While n-hexane extract fraction, the resulting eluental legedsesquiterpene Rf 0.49; 0.8,and 0.99.


2021 ◽  
Vol 37 (2) ◽  
pp. 426-432
Author(s):  
Shahbaz Khan ◽  
Harpreet Singh ◽  
Arun K Mishra ◽  
Najam Ali Khan

The present work includes extraction of Betula alnoides bark using ethyl acetate as a solvent, preliminary phytochemical test, quantification of phytochemicals and quantification of lupeol in Betula alnoides by High Performance Thin Layer Chromatography (HPTLC) instrument along with the assessment of the antimicrobial potential of Ethyl Acetate Extract (EAE). The marc obtained after defatting of the coarsely powdered crude drug in Petroleum ether (60-80) was extracted using ethyl acetate. Afterward, preliminary phytochemical tests were done. For High Performance Thin Layer Chromatography (HPTLC), the solvent used was n-hexane: ethyl acetate (8:2 v/v) and scanning was performed at wavelength 254 nm. EAE was screened for antimicrobial potential. The extraction yield was 3.45% w/w. The result of the phytochemical analysis confirmed the presence of some important phytochemicals in EAE. A clear and resolved peak of lupeol was observed at Rf 0.61. The developed method was validated as per ICH guidelines. The concentration (%) of the marker compound (lupeol) was found to be 0.0168. Disk diffusion method using Staphylococcus aureus, Pseudomonas aeruginosa and Bacillus subtilis as bacterial strains and Candida albicans, Aspergillus flavus and Epidermophyton floccosum as fungal strains against ciprofloxacin (for antibacterial activity) and fluconazole (for antifungal activity) as standard drugs was employed. The finding suggested that EAE possess significant antibacterial and antifungal activity when comparison was made with standard drugs. The proposed elucidated mechanism behind this action may be due to the presence of triterpenoids in EAE.


2015 ◽  
Vol 20 (2) ◽  
pp. 167 ◽  
Author(s):  
Ira Arundina ◽  
Theresia Indah Budhy S. ◽  
Muhammad Luthfi ◽  
Retno Indrawati

Karsinoma sel skuamosa rongga mulut merupakan jenis kanker yang paling sering ditemukan di rongga mulut. Faktor risiko utama terjadi keganasan di rongga mulut meliputi riwayat serta kebiasaan mengkonsumsi tembakau dan atau alkohol. Tanaman sudamala (Artemisia vulgaris L.) sering digunakan di masyarakat sebagai anti tumor pada organ pencernaan termasuk di rongga mulut, namun belum ada penelitian tentang bahan aktif yang berperan sebagai anti kanker di rongga mulut. Banyak didapatkan spesies dari genus Artemisia, sedangkan yang banyak tumbuh di Indonesia adalah spesies Artemisia vulgaris L. Tujuan penelitian ini adalah untuk menjelaskan identifikasi menggunakan Kromatografi Lapis Tipis (KLT) dari sudamala. Penelitian meliputi ekstraksi sudamala, identifikasi ekstrak sudamala, fraksinasi sudamala menggunakan Kromatografi Kolom Vakum dan identifikasi dari fraksi sudamala menggunakan Kromatografi Lapis Tipis (KLT). Ekstrak heksan sudamala yang dilakukan fraksinasi menggunakan n-heksan: etil asetat menghasilkan 11 fraksi. Fraksi n-heksan: etil asetat (3:7,v/v) dari sudamala yang teridentifikasi menggunakan Kromatografi Lapis Tipis (KLT) mengandung terpenoid.Identification of Sudamala ( Artemisia vulgaris L.) Thin Layer Chromatography. Oral squamous cell carcinoma is the type of cancer which is most frequently found in oral cavity. The primary risk factor of malignancy in oral cavity includes the habit of consuming tobacco and or alcohol. The plant sudamala (Artemisia vulgaris L.) is often used in the community as anti-tumor in digestive organ, including in oral cavity. However, there have been no studies on active ingredients playing the role as anti-cancer in oral cavity. The species are mostly from the genus Artemisia, while those generally growing in Indonesia are the species Artemisia vulgaris L. The objective of this study is to explain the identification by TLC of sudamala. The study was sudamala extraction, identification of sudamala extract, sudamala fractionation with Vacuum Column Chromatography and identification of sudamala fractionation with TLC (Thin Layer Chromatography). The result shows that the fractionation using hexane extract resulted in 11 fractions of n-hexane: ethyl acetate. The conclusion of this study is that the fraction of n-hexane: ethyl acetate (3:7, v/v) sudamala (Artemisia vulgaris L.) identified contains terpenoids compounds.


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