Extraction of trifluralin from acetonitrile solutions

Results of extraction of trifluralin from an aqueous acetonitrile solution using various organic solvents are presented. The degree of extraction was shown to depend on the nature of extractant and the water/acetonitrile ratio. An optimal electrolyte and the degree of saturation of the water-acetonitrile layer with this electrolyte were selected. The highest efficiency of extraction was achieved by using water-saturated ethylacetate as an extractant. The indices of extraction were calculated as necessary for the isolation of a given amount of trifluralin from aqueous acetonitrile (4:1) solutions with the solvents considered in the present study.     

Synthesis of 4-methyl-5-arylpyrimidines and 4-arylpyrimidines: route specific markers for the Leuckardt preparation of amphetamine, 4-methoxyamphetamine, and 4-methylthioamphetamine

General synthetic routes to 4-methyl-5-arylpyrimidines and 5-arylpyrimidines are described. 4-Benzylpyrimidine, 4-methyl-5-phenylpyrimidine, 4-(4-methoxybenzyl)pyrimidine, and 4-methyl-5-(4-methoxyphenyl)pyrimidine have been positively identified as route-specific by-products in the Leuckardt preparations of amphetamine and 4-methoxyamphetamine.Using headspace solid phase microextraction (SPME) 4-(4-methoxybenzyl)pyrimidine and 4-methyl-5-(4-methoxyphenyl)pyrimidine have been identified in illicit tablets containing 4-methoxyamphetamine. This is an indication that illicit laboratories use the Leuckardt method for the preparation of 4-methoxyamphetamine.Flatliner tablets containing 4-methylthioamphetamine have been screened for the presence of 4-(4-methylthiobenzyl)pyrimidine and 4-methyl-5-(4-methylthiophenyl)pyrimidine using both headspace and aqueous phase SPME. As these pyrimidines were not detected it would appear likely that illicit laboratories are not using the Leuckardt method for the preparation of 4-methylthioamphetamine.     

Extraction of lambda-cyhalothrin from aqueous dioxan solutions

The results of extraction of lambda-cigalotrin from dioxan aqueous solutions by hydrophobic organic solvents are presented. It is shown that the degree of extraction depends on the nature of the extractant, the water to dioxan ratio, and saturation of the water-dioxan layer with the electrolyte. The highest efficiency of lambda-cigalotrin extraction was achieved using chlorophorm as a solvent under desalination conditions. The extraction factor was calculated necessary to obtain the desired amount of lambda-cigalotrin from the water-dioxan solution (4:1) with the help of the extractants being used.     

Optimization of the conditions for extracting metronidazole with organic solvents]

Optimal conditions of metronidazole extraction from aqueous solutions by different solvents using a mathematical method of experiment planning (latin square) were studied. It was stated that optimal conditions of metronidazole extraction from aqueous solutions were: extraction time (5 min.), pH medium-6, extractant-isoamyl spirit in saturation of aqueous phase with ammonium sulfate.     

Extraction of nitrobenzene and its metabolite 3-aminohydroxybenzene from water solutions

The article presents the results of nitrobenzene and 3-aminohydroxibensene extraction from aqueous solutions by means of five organic solvents. The following factors influence on the extraction degree is shown: the nature of the extracting agent, aqueous phase pH, saturation of some extracting agents with water. The number of extractions for isolation of the necessary quantities of the compounds studied is calculated.     

DNOC extractability from aqueous solutions

Extractability of 2-methyl-4,6-dinitrophenol from aqueous solutions by means of different organic solvents was studied. Effect of solvent nature, pH medium and extractant saturation with water was noted.     

Extraction of 2-nitroaniline and 2-nitro-4-methylaniline from aqueous solutions

Results of extraction of 2-nitroaniline and 2-nitro-4-methylaniline from aqueous solutions with organic solvents are shown to depend on the nature of extractants, pH of the aqueous phase, its saturation with water and electrolytes. The optimal conditions for the extraction of the compounds of interest are created by using water-saturated ethylacetate as the extractant at a pH value in the range from 1.0 to 12.0. The rate of extraction was calculated necessary to remove the desired amounts of 2-nitroaniline and 2-nitro-4-methylaniline from aqueous solutions using the above solvents.     

Extraction of 2-amino-4-nitrophenol and 4-phenylphenol from aqueous solutions

The authors provide the results of extraction of 2-amino-4-nitrophenol and 4-phenilphenol from aqueous solutions by five organic soluvants. The dependence of the extraction degree on some factors (nature of extragent, pH of aqueous phase medium, extragents saturation with water) was established. Necessary extraction rate for isolation of preset quality of the test substances was calculated.     

Features of extracting phenol and 4-methylphenol from aqueous solutions

Phenol and 4-methylphenol were extracted from aqueous solutions by 5 organic solvents. The degree of extraction depended on such factors as type of extracting agent, pH of aqueous phase, and water saturation of extracting agent. The necessary number of extractions for obtaining the preset volumes of studied compounds is calculated.     

Solid-phase cation exchange extraction of basic drugs from the urine of racing greyhounds

The extraction of basic drugs from the urine of racing greyhounds has been carried out for many years using solvent extraction. This paper describes an extraction method that utilises a cation exchange column. Fourteen basic drugs were introduced onto the column in their ionised form, washed with organic and aqueous solvents and eluted with basic methanol. Three drugs, cyclizine, procaine and quinine were determined in authentic samples from racing greyhounds. A comparison of the solid-phase method with liquid-liquid extraction showed an increase in the efficiency of extraction and a reduction in both the time and cost incurred. The method requires a minimal volume of sample and solvent, little glassware and is easily automated.     

The extraction of deoxypeganin from aqueous solutions with organic solvents]

Studies of deoxypeganin extraction with various organic solvents have shown that up to 88% of the agent can be easily extracted by chloroform if the medium pH values are 11-12. The presence of electrolytes in deoxypeganin aqueous solutions does not influence the degree of the agent extraction with organic solvents.     

Isolation, extractive concentration, and determination of caffeine in the studies of blood plasma

The optimal conditions for the isolation of caffeine from human blood by means of acetone extraction are described with special reference to the peculiarities of extraction from aqueous solutions. The possibility of concentration and purification of caffeine from blood plasma using acetone and aceton-chlorophorm mixture (2:8) as the solvents is illustrated. In addition, purification by silica-gel thin layer chromatography is discussed. Thin layer chromatography, UV-spectrophotometry, and high performance liquid chromatography are considered as potential methods for the identification and quantitative determination of caffeine.     

A simple method of DNA extraction and STR typing from urine samples using a commercially available DNA/RNA extraction kit

We devised a simple DNA extraction procedure suitable for STR typing of urine sample. Use of a commercially available DNA/RNA extraction kit equipped with a silica-gel-based membrane made it possible to omit the recovery of urinary nucleated cells by sedimentation before the extraction. Successful genotyping of the TH01, HumTPO and multiplex STRs was achieved using aliquots of urine as small as 100 microL. Furthermore, application of this DNA extraction procedure to frozen urine samples provided STR allele results comparable to results obtained from fresh samples. Therefore, this extraction procedure is considered to be effective for STR typing of urine samples in both the frozen and aqueous state. Furthermore, addition of sodium azide to fresh urine samples prolonged their storage duration even at room temperature.     

The comparative characteristics of the extractive capacity of solvents in removing aminazine from liver tissue

Comparative assessment of extractive ability of some solvents with different physical and chemical properties is presented. Use of amphiphilic solvent acetone to isolate aminazine gave higher results. Experimental works (on dogs) showed that use of aqueous acid solutions for aminazine extraction in chemical toxicological investigation is unsuitable.     

An aqueous-organic extraction method for the isolation and identification of psilocin from hallucinogenic mushrooms

A simple aqueous extraction method for the isolation and identification of psilocin from Psilocybe cubensis mushrooms is reported. This method employs a dephosphorylation of the phosphate ester to psilocin, which facilitates a greater product yield and simplifies identification. Psilocin extracted by this method is sufficiently concentrated and free of cocontaminants to allow identification by infrared spectroscopy and gas chromatography/mass spectrometry.     

Detection and confirmation of fentanyls in high clay-content soil by electron ionization gas chromatography-mass spectrometry

Detection of illicit drugs in the environment, particularly in soils, often suggests the present or past location of a clandestine production center for these substances. Thus, development of efficient methods for the analysis and detection of these chemicals is of paramount importance in the field of chemical forensics. In this work, a method involving the extraction and retrospective confirmation of fentanyl, acetylfentanyl, thiofentanyl, and acetylthiofentanyl using trichloroethoxycarbonylation chemistry in a high clay-content soil is presented. The soil was spiked separately with each fentanyl at two concentrations (1 and 10 μg/g) and their extraction accomplished using ethyl acetate and aqueous NH₄OH (pH ~ 11.4) with extraction recoveries ranging from ~56% to 82% for the high-concentration (10 μg/g) samples while ranging from ~68% to 83% for the low-concentration (1 μg/g) samples. After their extraction, residues containing each fentanyl were reacted with 2,2,2-trichloroethoxycarbonyl chloride (Troc-Cl) to generate two unique and predictable products from each opioid that can be used to retrospectively confirm their presence and identity using EI-GC-MS. The method's limit of detection (MDL/LOD) for Troc-norfentanyl and Troc-noracetylfentanyl were estimated to be 29.4 and 31.8 ng/mL in the organic extracts. In addition, the method's limit of quantitation for Troc-norfentanyl and Troc-noracetylfentanyl were determined to be 88.2 and 95.5 ng/mL, respectively. Collectively, the results presented herein strengthen the use of chloroformate chemistry as an additional chemical tool to confirm the presence of these highly toxic and lethal substances in the environment.     

Comparison of molecularly imprinted solid-phase extraction (MISPE) with classical solid-phase extraction (SPE) for the detection of benzodiazepines in post-mortem hair samples

This preliminary study compares the benzodiazepine results for 10 post-mortem scalp hair samples using a classical solid-phase extraction (SPE) and a molecularly imprinted solid-phase extraction (MISPE) system. The hair samples selected for testing were from drug-related deaths where a positive benzodiazepine blood result was obtained. Samples were decontaminated with 0.1% sodium dodecyl sulfate, distilled water and dichloromethane, incubated overnight in methanol/25% aqueous ammonium hydroxide (20:1), extracted by SPE or MISPE and subsequently analysed by liquid chromatography-tandem mass spectrometry (LC-MS-MS). Both extraction methods detected diazepam, nordiazepam, oxazepam, temazepam and nitrazepam in the samples. Diazepam was detected in a greater number of samples using MISPE due to both its lower limit of detection (LOD) and higher extraction recovery as a result of excellent molecular recognition of the template (diazepam) imparted by the imprinting process. The selective recognition of two diazepam analogues, nordiazepam and oxazepam, was demonstrated using MISPE since they were also detected in a greater number of samples. In contrast, another diazepam analogue, temazepam, was detected in a greater number of samples using SPE since the LOD using this extraction was lower than with MISPE. Nitrazepam was detected in one sample using both extraction methods. Overall the MISPE and SPE hair results were in good qualitative agreement. For the samples, where both extraction methods detected nordiazepam, temazepam and oxazepam, the concentrations were always higher for SPE. This is probably due to the MIP procedure producing extracts with fewer matrix interferences than the extracts produced using the classical SPE method. MISPE could be used as a complementary method to classical SPE for the analysis of benzodiazepine positive hair samples collected from chronic users.     

Methods for detecting diazoline in chemicotoxicological studies]

New specific methods of diazolin detection by microcrystalline and chromogenic reactions as well as by thin-layer sorbent chromatography were developed. These methods were used to detect diazolin, isolated from biological object by water acidified with oxalic acid. It was stated that diazolin is detectable in chlorophorm extraction obtained both from acidic and from alkaline aqueous solutions.     

Cloud point extraction coupled with back extraction: a green methodology in analytical chemistry

Recently, cloud point extraction (CPE) coupled with back extraction (BE) has been suggested as a promising alternative to liquid-liquid extraction. In CPE, non-ionic surfactants in aqueous solutions form micelles and the solution becomes turbid when heated to the cloud point temperature. Microwave- or ultrasonic-assisted BE can be performed after CPE and before injection of the sample for instrumental analysis by ultraviolet-visible spectroscopy, high-performance liquid chromatography, gas chromatography, gas chromatography-mass spectrometry, or liquid chromatography-mass spectrometry. This article reviews selected published scientific research on the application of CPE-BE to the determination of alkaloids, drugs and organophosphorus compounds from several complex matrices. This method could be scaled-up for use in forensic science.     

The extraction and infrared identification of gamma-hydroxybutyric acid (GHB) from aqueous solutions

The chemical analysis of gamma-hydroxybutyric acid (GHB) in most forensic laboratories is complicated by the highly polar nature of the GHB molecule, which makes it unsuitable for direct analysis by gas chromatography (GC). Consequently, a popular analytical approach is to convert GHB into the corresponding lactone or a derivative compound that is then identified by mass spectrometry employed in conjunction with GC (GC/MS). An alternative approach is presented here where GHB may be isolated as a free acid specie from complex aqueous solutions employing a liquid-liquid extraction technique. This approach can yield a relatively pure residue of GHB that presents an infrared transmission spectrum that is sufficiently distinct for identification purposes. Infrared spectroscopy (IR) is a very popular technique that is available to most crime laboratories. The liquid-liquid extraction behavior of GHB is examined in detail and the uniqueness of the infrared spectrum is discussed.