Determination of Biphenyl in Citrus Fruits by Quantitative Thin-Layer Chromatography

Abstract

Residues of the fungicide biphenyl in citrus fruits have been determined by direct scanning of spots on phosphor-impregnated high performance silica gel TLC plates under UV light. Biphenyl was separated from fruit tissue by steam liquid-liquid extraction. Recoveries from spiked samples ranged from 92–99% at 100, 50, and 10 ppm levels. The precision of the TLC determination and overall procedure are shown to be adequate for residue analysis.     

Determination of Chlorpyrifos and its Metabolite 3,5,6-Trichloro-2-Pyridinol in Tap Water and Bananas by Quantitative TLC on Preadsorbent Silica Gel

Abstract

Chlorpyrifos insecticide and its metabolite TCP were determined in tap water and banana samples by TLC of extracts on preadsorbent silica gel layers, detection with silver nitrate reagent, and densitometric scanning. Cleanup steps were required for the fruit sample extracts. Recovery of chlorpyrifos from tap water at 5 ppb averaged 87.5% and from banana at 0.05 ppm was 84.6%. Recovery of TCP from water at 5 ppb averaged 84.0% and from banana at 0.05 ppm was 86.8%. The sensitivity and precision of the method were shown to be adequate for routine residue analysis.     

Analysis of Phosmet and Azinphos-Methyl in Apples by High-Performance Liquid Chromatography

Abstract

A high-performance liquid chromatography (HPLC) method has been developed to analyze two organophosphate insecticides (phosmet and azinphosmethyl) in apples. The procedure includes a novel extraction whereby whole apples are sonicated for 2 min in 100 ml of MeOH to remove the pesticides. Reversed-phase HPLC separation was accomplished with an Ultremex C18 column and acetonitrile:methanol:water as the eluent. Detection was at 224 nm for phosmet and 300 nm for azinphos-methyl. For both pesticides the limit of detection was 0.5 ppb and the linearity was from 1 to 405 ng injected. Average recoveries were 80% for phosmet and 86% for azinphos-methyl. Thirteen apple varieties comprising 240 apples were analyzed from supermarkets and roadside stands for phosmet (amount found ranged from none detected to 1233 ppb) and azinphos-methyl (amount found ranged from none detected to 388 ppb). Confirmation of phosmet and azinphos-methyl was made by UV spectral scans.     

The Thin-Layer Chromatographic Separation of Halogenated Fumigants as Ammonium Halides and Their Subsequent Determination by Meca

Abstract

A method is described for the determination of several pesticides containing bromine and chlorine by molecular emission cavity analysis (MECA). The pesticides were decomposed in an oxygen flask and the combustion products dissolved in aqueous ammonia. The ammonium halides were separated by TLC using microcrystalline cellulose adsorbent. After scraping from the TLC plates and dissolving in water the separated components were quantitated by MECA using either the InBr (Λ_max = 376 nm) or the InCl (Λ_max = 360 nm) emission bands. Recoveries of over 96% were obtained. Soils fortified with l, 2-dibromo-3-chloropropane at levels of 5–25 ppm were extracted using shaking and distillation procedures. Subsequent analysis showed that the shaking extraction gave a recovery of 92% compared to 85% from acid refluxing.     

Liquid Chromatographic Determination of Dimetridazole and Ronidazole in Feeds

Abstract

A simple high performance liquid chromatographic (HPLC) procedure for the simultaneous determination of dimetridazole and ronidazole in turkey feeds is described. The drugs are extracted from feeds by carbon-tetrachloride/dimethylformamide (80:20) at 60°C during 30 mn and the extract is subjected to a partition by water. After centrifugation the eluate is chromatographed on a reverse phase column with ultaviolet detection at 316 nm. Recoveries from samples fortified at levels 2.02 to 7.07 ppm for ronidazole and 2.01 to 7.03 for dimetridazole were 99,6% ± 1,4 and 95,3% ± 1,8 (mean ± standard deviation), respectively.     

Liquid Chromatographic-Electro-Chemical Technique for Determination of Ethylenethiourea Residues

Abstract

A high performance liquid chromatographic-electrochemical (HPLC-EC) technique was developed to selectively determine ethylenethiourea (ETU) at residue levels without derivatization. ETU was eluted from a C-8 column with water, a phosphoric acid electrolyte solution was added to the column eluate, and then ETU was detected with an electrochemical detector containing a Au/Hg working electrode. The HPLC-EC system produced a sharp chromatographic peak for ETU that was detected by the Au/Hg electrode at an applied potential of +0.36 V. With detector sensitivity adjusted so that 10 ng ETU produced a 50% full scale deflection peak (1% baseline noise), the detector's response was linear from 2 to 400 ng ETU. No peaks were observed in potato and spinach controls, and only small apparent ETU peaks of 7 and 3 ppb, respectively, were found in apple and grape controls. Detector response was equivalent to 90% of actual ETU added (0.1 ppm) to purified spinach extracts. Crop coextractives from apples, grapes and potatoes did not affect detector response to ETU at the 0.1 ppm fortification level.     

Determination of Allantoin in Drug Preparations by Quantitative High Performance TLC

Abstract

A densitometric TLC method was developed for the quantification of allantoin in creams and suppositories used to treat vaginal infections. Allantoin was extracted with water at elevated temperature, diluted to a known volume, and separated by HP silica gel TLC. Allantoin was detected by spraying with p-dimethylamine-benzaldehyde reagent. The absorption of standards and samples was compared by in situ scanning. Recoveries of allantoin from authentic samples ranged from 96–102%, except for one sample that assayed high. The accuracy of the method was demonstrated by standard addition analysis of this sample.     

Determination of Sulfanilamide and Sulfisoxazole in Drug Preparations by Quantitative High Performance TLC

Abstract

A densitometric TLC method was developed for quantification of sulfanilamide and sulfisoxazole in creams, supppositories, and tablets. The sulfas were extracted into acidic ethanol, diluted to an appropriate volume, and separated by silica gel HPTLC. The fluorescence quenching of the sulfa zones in samples and standards was compared by in situ scanning. Recoveries of the drugs from authentic samples ranged from 96–105%. Recoveries from products with old expiration dates were low. Identity of the sulfa drugs in products was confirmed by application of fluorescamine and Bratton-Marshall detection reagents.     

Determination of Triazine and Chlorophenoxy Acid Herbicides in Natural Water Samples By Solid Phase Extraction and Quantitative Thin Layer Chromatography

Abstract

Atrazine, simazine, 2, 4-D, silvex, and 2, 4, 5-T, were determined in natural water samples at 10 ppb levels by solid phase extraction on disposable C₁₈ columns and TLC on preadsorbent silica gel layers impregnated with AgNO₃, exposure to UV light, and densitometric scanning. Recoveries ranged from 70 to 88% for the triazines and 93 to 100% for chlorphenoxy acid herbicides, with average CV values of 7 to 8%. Solid phase extraction proved to be an advantageous alternative to classical liquid-liquid partition for the analysis of water for these compounds by quantitative TLC.     

Residue Analysis of Propionylbrassinolide in Fruit and Vegetables by GC–MS

A rapid and simple method for the determination of propionylbrassinolide residues in tomatoes, apples and grapes using GC–MS is reported. Samples were extracted with acetonitrile, and the extracts were analyzed without any further clean-up. The results showed good linearity (r ² > 0.99) with standard solutions over the concentration range of 0.5–50 mg L⁻¹. The LODs and LOQs of propionylbrassinolide were 0.15 and 0.5 mg kg⁻¹ in all samples. Recoveries were in the range of 81.9–111.2%, with corresponding RSDs of 4.6–12.9% for three fortified levels. Intra- and inter-day RSDs were in the ranges of 1.5–14.2% and 5.3–15.6%. It was demonstrated that the proposed method is simple and efficient, and particularly suitable for detecting propionylbrassinolide residues in fruit and vegetables.

     

An accurate and reproducible method for simultaneous determination of four flavonoids in EtOAc extracts from Sophora flavescens Ait. in rat plasma based on UHPLC Q‐Exactive Mass spectrometry: Application to a pharmacokinetics study

In previous studies, it was revealed that ethyl acetate (EtOAc) extracts from Sophora flavescens Ait. improved glucose tolerance, reduced hyperglycemia, and restored insulin levels in diabetic patients. The aim of this study was to develop an accurate and sensitive UHPLC–MS method for simultaneous determination of flavonoids in EtOAc extracts of Kushen in rat plasma. Ethyl acetate–acetonitrile (2:1) was selected as the solvent to extract the four flavonoids from rat plasma. A BEH C₁₈ column (2.1 mm × 100 mm, 1.7 μm) with a C₁₈ guard cartridge was chosen as the separation plant using a gradient elution with acetonitrile (solvent A) and 0.1% formic acid (solvent B) in water. For all four analytes, the method showed good linearity (r² > 0.991) in 1–500 ng/mL. The inter‐ and intra‐day accuracy ranged from ?13.78 to 7.19%, and the precision (RSD) was <8.75%. Recoveries of all four flavonoids ranged from 85.9 to 101.3%. According to the results of multitarget pharmacokinetic studies, four active flavonoids in EtOAc extracts from Kushen have similar absorption kinetics but very different metabolic kinetics, and a double peak phenomenon was observed in the concentration–time curve of norkurarinone, which is different from the previous study. In conclusion, detection and multitarget pharmacokinetic studies successfully determined active flavonoids after oral administration of EtOAc extracts from Kushen by an efficient, sensitive and selective UHPLC–MS method, and the results may provide a foundation for future studies of Kushen.     

Monitoring of Polychlorinated Biphenyls in Surface Water Using Liquid Extraction,GC/MS,and GC/ECD

Abstract

A rapid and reliable analytical method, at trace level concentration was developed and validated for monitoring polychlorinated biphenyls (PCBs) in Jordanian surface water. The method combines the advantage of liquid extraction together with gas chromatography‐mass spectrometry (GC/MS) and gas chromatography‐electron capture detector (GC/ECD). The performance of the method was evaluated by analyzing certified reference material (CRM) of the analytes and applied on real water samples collected from different sites in Jordan. A mixture of 60∶40 dichloromethan‐petroleum ether was chosen as a convenient binary solvent for liquid–liquid extraction. The GC conditions for GC/MS were optimized using He as a carrier gas, temperature programming, and chlorpropham as an internal standard (IS).

The conditions for GC/ECD were performed using N₂ gas and a temperature program from 160 to 280°C with different increasing rates. The method of GC/MS in the selective ion mode (SIM) gave linear relationships for all PCBs tested between 0.60–6.0 µg/l with R ²=0.9934 (n=7×18). Recoveries from spiked water samples ranged between 87.6 and 91.4%. The mean accuracy and precision obtained were 4.9% and 2.16%, respectively. The mean of detection limit was 0.14±0.04 µg/l. In GC/ECD, linear relationships for all PCBs examined over the range of 0.3–2.4 µg/l was verified as characterized by a linear regression equation and correlation coefficient, R ²=0.9915 (n=12). The average precision and accuracy were 4.86% and 5.21%, respectively. Analyses results clarified that none of the examined Jordanian water samples contained any of the searched for PCBs within the detection limit achieved.     

Residue Analysis of Propionylbrassinolide in Fruit and Vegetables by GC–MS

A rapid and simple method for the determination of propionylbrassinolide residues in tomatoes, apples and grapes using GC–MS is reported. Samples were extracted with acetonitrile, and the extracts were analyzed without any further clean-up. The results showed good linearity (r ² > 0.99) with standard solutions over the concentration range of 0.5–50 mg L^?1. The LODs and LOQs of propionylbrassinolide were 0.15 and 0.5 mg kg^?1 in all samples. Recoveries were in the range of 81.9–111.2%, with corresponding RSDs of 4.6–12.9% for three fortified levels. Intra- and inter-day RSDs were in the ranges of 1.5–14.2% and 5.3–15.6%. It was demonstrated that the proposed method is simple and efficient, and particularly suitable for detecting propionylbrassinolide residues in fruit and vegetables.     

Determination of fenthion and fenthion-sulfoxide, in olive oil and in river water, by square-wave adsorptive-stripping voltammetry

Square-wave adsorptive-stripping voltammetry technique has been used to develop a method for the determination of fenthion in olive oil. Due to the fact that fenthion does not give any electrochemical signal at mercury electrode, the method has been based on a previous oxidation of fenthion to its metabolite, fenthion-sulfoxide, by using KMnO₄. The metabolite gives rise to a peak due to an adsorptive-reductive process at −0.786 V. Fenthion is isolated from olive oil by carrying out a solid–liquid extraction procedure using silica cartridge, followed by a liquid–liquid partitioning with acetonitrile. The detection limit in olive oil is 78.8 ng g⁻¹ and recoveries for four levels of fortification are ranged from 85% to 109%. On the other hand, it has been developed a method for the simultaneous determination of fenthion and its metabolite fenthion-sulfoxide, in river water. Pesticides are isolated from water by carrying out a liquid–liquid partitioning with trichloromethane. The detection limits are 0.41 ng g⁻¹ and 0.44 ng g⁻¹, for fenthion and fenthion-sulfoxide, respectively. Recoveries for three levels of fortification are ranged from 96% to 103% for fenthion and 94% to 104% for fenthion-sulfoxide.     

High Performance Liquid Chromatographic Determination of Neomycin in Milk Using a Hisep Column

Abstract

A high performance liquid chromatographic (HPLC) method for the determination of neomycin in milk is described. Milk is passed directly through an amberlite CG-50 ion exchange resin column, and the neomycin which is retained on the column is derivatized with ortho-phthalaldehyde (OPA) reagent. The derivatized neomycin is eluted from the column with potassium borate buffer/methanol and analyzed by HPLC. A HISEP HPLC column with fluororoetric detection was used. Recoveries ranged from 94 to 102% in samples fortified between 0.1 to 5ppra levels. The detection limit is 50ppb.     

Screening and characterization of medicinal plants extracts with bactericidal activity against Streptococcus mutans

Abstract

The aim of the present study was to perform a screening of extracts obtained from 15 medicinal plants using water (at 25 and 90?°C) or ethanol (at 25?°C), to bactericidal activity against cariogenic S. mutans ATCC 25175, as well as to carry out the preliminary phytochemical characterization of the extracts and HPLC/MS assay for selected extracts. The extractions were carried out for 5?h at 400?rpm. Only five from 45 tested extracts were selected based on their antibacterial activity. The IC₅₀ varied from of 28?ppm for Quercus ilex up to 250?ppm for Jatropha dioica. Different polyphenolic and quinic acids, flavonoids, anthocyanin or tyrosol were identified by HPLC/MS in selected extracts from Rosa gallica L., Jatropha dioica Sessé, Mimosa tenuiflora (Willd.) Poir, Quercus ilex L., and Solanum nigrum. The obtained results confirm that selected extracts are good candidates to be used for cariogenic bacteria control.     

Determination of clethodim and its oxidation metabolites in crops by liquid chromatography with confirmation by LC/MS

A method was developed for determination of the herbicide clethodim (C0) and its oxidation metabolites clethodim sulfoxide (C1) and clethodim sulfone (C2) in agricultural products. Upon extraction, both C0 and C1 were oxidized to C2 by m-chloroperoxybenzoic acid, and C2 was determined by liquid chromatography (LC). The C2 peak was confirmed by liquid chromatography/mass spectrometry (LC/MS) with electrospray ionization (ESI). Recoveries of C0 from radish, tomato, onion, sweet potato, kidney bean, carrot, cabbage, and lettuce ranged from 91 to 118% following fortification at 0.05-1.0 ppm. The detection limit of C2 in crops was 0.01 ppm (S/N > 3). The fortified samples of onion, sweet potato, kidney bean, and carrot were confirmed by LC/MS (ESI), and the peak of C2 was detected.     

A Direct Spectrofloorimetric Method for the Determination of B-Naphthoxyacetic Acid Residues in Strawberries

Abstract

β-naphthoxyacetic acid (NOA) residues in strawberries have been determined in acetone extracts using direct, first and second derivatives with spectrofluorimetric detection, without clean-up procedures needed. Solvent effects on the spectral characteristics of NOA solutions and their influences on the sensitivity of its variables and instrumental parameters are also studied. A detection limit of 1.14 ng/ml was achieved using the first derivative approach. Strawberries were fortified at different NOA concentrations (10 to 90 ng/ml). Recoveries averaged 87.2% (range 80.16–98.53) at the lower fortification level and 98.36% (range 97.54–99.63) for the higher fortification level.     

Effect of Water and Ethanol Extracts from Hericium erinaceus Solid-State Fermented Wheat Product on the Protection and Repair of Brain Cells in Zebrafish Embryos

Extracts from Hericium erinaceus can cause neural cells to produce nerve growth factor (NGF) and protect against neuron death. The objective of this study was to evaluate the effects of ethanol and hot water extracts from H. erinaceus solid-state fermented wheat product on the brain cells of zebrafish embryos in both pre-dosing protection mode and post-dosing repair mode. The results showed that 1% ethanol could effectively promote zebrafish embryo brain cell death. Both 200 ppm of ethanol and water extracts from H. erinaceus solid-state fermented wheat product protected brain cells and significantly reduced the death of brain cells caused by 1% ethanol treatment in zebrafish. Moreover, the zebrafish embryos were immersed in 1% ethanol for 4 h to cause brain cell damage and were then transferred and soaked in the 200 ppm of ethanol and water extracts from H. erinaceus solid-state fermented wheat product to restore the brain cells damaged by the 1% ethanol. However, the 200 ppm extracts from the unfermented wheat medium had no protective and repairing effects. Moreover, 200 ppm of ethanol and water extracts from H. erinaceus fruiting body had less significant protective and restorative effects on the brain cells of zebrafish embryos. Both the ethanol and hot water extracts from H. erinaceus solid-state fermented wheat product could protect and repair the brain cells of zebrafish embryos damaged by 1% ethanol. Therefore, it has great potential as a raw material for neuroprotective health product.     

Determination of Cyclohexylamine in Water by Solid Phase Extraction and Quantitative High Performance Thin Layer Chromatography

Abstract

Cyclohexylamine (CHA) was isolated from water by solid phase extraction on a C₁₈ microcolumn. The CHA in the column eluate was chromatographed on a high performance preadsorbent silica gel layer, detected with ninhydrin reagent and exposure to UV light, and quantified by reflectance scanning. Recovery from fortified distilled water samples at 10 ppm averaged 95.0% and at 1 ppm averaged 94.9%. Quantitative recoveries from tap water at 10 ppm and from lake water at 1 ppm were also demonstrated. Other boiler water additives permitted by FDA do not interfere.