Liquid Extraction Method Research Articles

The Removal of Platinum Group Metals, Cs, Se, and Te from Nuclear Waste Glass Using Liquid Sb Extraction and Phase Separation Methods.

Recovery of platinum group metals (PGMs: Pd, Ru, Rh), Cs, Se, and Te from molten borosilicate glass containing simulated high level radwaste through the combination of liquid metal extraction and phase separation method under reductive heat-treatment was studied. In this process, the PGMs were extracted in recovered liquid metal phase, where Sb and Bi metals were used as the collecting metals. Meanwhile, Cs, Se, and Te were enriched in the phase separated potassium-rich materials on glass surface, which were extracted by water. The type of liquid metals had profound influence on the extraction behaviors of PGMs and other fission products from the glass melt. As a result, except the near extraction efficiency of Pd, Sb showed higher affinity for Ru and Rh than Bi metal. The higher phase separation efficiency of potassium-rich materials led to the higher extraction efficiencies of Cs, Se, and Te in liquid Sb extraction than Bi. Among the examined conditions, using liquid Sb extraction, the Pd, Ru, and Rh extraction efficiencies were 78.6%, 62.1% and 100% in liquid Sb metal phase, and 93.76% of Cs, 60.4% of Se, and 23.65% of Te in leachate were obtained.

Microbial conversion of vanillin from ferulic acid extracted from raw coir pith

Coir pith, an agro-industrial residue, is resistant to natural degradation, and its accumulation causes environmental pollution. Ferulic acid, a precursor of vanillin, was extracted from the raw coir pith by chemical pre-treatment such as alkaline hydrolysis, acidification, and liquid–liquid extraction method. The obtained ferulic acid (1.2 g/50 g) was analysed using high-performance liquid chromatography (HPLC) and used as a substrate for biotransformation by Aspergillus niger to vanillic acid, which, in turn, was fermented by using Phanerochaete chrysosporium to vanillin. The quantity of vanillic acid detected by HPLC on the third day of incubation was 0.773 g/L, while the optimal yield of vanillin on the subsequent third day of incubation was 0.628 g/L. Thus, the chemical extraction of ferulic acid from coir pith ensued bioconversion into vanillin. These products are highly valuable and economical to be used in industries such as pharmaceuticals, health, cosmetics, and neutraceuticals.

Removal of toxic heavy metals, phenolic compounds and textile dyes from industrial waste water using phosphonium based ionic liquids

This article focused on a comprehensive result of the development of three phosphonium based room temperature ionic liquids (RTILs) of same cation, trihexyltetradecylphosphonium ([PC6C6C6C14]), with different organic or inorganic anions viz. [Cl-] chloride dicyanamide [-N(CN)2−] and bis (trifluoromethyl sulfonyl) amide [-NTf2−] in extraction processes of toxic textile dyes as rhodamine B, methylene blue, methyl orange, malachite green, alizarin red S and congo red dyes from their aqueous solution, harmful heavy metals include As, Cr, Cd, Cu, Zn, Pb and Hg from their standard solutions AS(NO3)3, Cr(NO3)3, Cd(NO3)2, Hg(NO3)2, Pb(NO3)2, Zn(NO3)2 & Cu(NO3)2 respectively and phenolic compounds from rice and cashew industrial waste water. In technological front, ILs revealed a potential ability for the removal of dyes, heavy metals and phenolic compounds owing to their hydrophobic nature on investigating via liquid –liquid extraction method. The effect of contact time, solution pH and initial concentration of dyes were investigated and the result show that adsorption of dyes increases with increasing contact time and gets maximum decolourisation at acidic pH and pH 7. The extraction process of heavy metals with the ILs were investigated and were assessed using the techniques UV–Visible spectroscopy and ICP-MS (Inductive Coupled Plasma Mass Spectroscopy). The three ILs showed best extraction efficiency (approx. 100%) for all heavy metals and the dyes using proposed methodology. UV–Visible Spectroscopy quantification method was employed to analyse extracted phenolic compounds. Screening results of phenolic compounds have shown that [PC6C6C6C14][Cl] IL exhibited the capacity intake of 100% efficiency from rice and cashew industrial waste water. The ILs were characterized with thermogravimetry (TGA) and from which, the samples showed a good thermal stability up to 573 K to project them as promising one for high temperature needs in various technological fronts. Toxicity risks of the three ILs and the textile dyes used were examined by in silico OSIRIS software calculations and the ILs were found to be non-toxic.

Sustainable Production of 5-Hydroxymethylfurfural from Pectin-Free Sugar Beet Pulp in a Simple Aqueous Phase System-Optimization with Doehlert Design

Waste solid residue from the hydrothermal extraction of pectin derived from sugar beet pulp was used as feedstock in the production of 5-hydroxymethylfurfural (5-HMF). The depolymerization of pectin-free sugar beet pulp (PF-SBP) to monosaccharides and their dehydration to 5-HMF were conducted in subcritical water using a batch reactor. The experimental design methodology was used in order to model the hydrothermal process and to optimize the operational parameters of the reaction, namely temperature and holding time. These parameters are required to achieve the highest yield of 5-HMF. The model predicts, in good agreement with experimental results (R2 = 0.935), an optimal yield of 5-HMF (of approximately 38% in relation to the cellulosic fraction content in the PF-SBP) at a temperature of 192.5 °C and a holding time of about 51.2 min. 5-HMF was successfully isolated from the reaction mixture using the liquid–liquid extraction method. The results are suitable for industrial upscaling and may become an incentive to introduce a new, environmentally friendly, uncomplicated, and efficient waste treatment method. The method would be used to treat products from the sugar refining industry, the treatment of which has proven to be problematic until now.

Salting‐out assisted liquid–liquid extraction method optimized by design of experiments for the simultaneous high‐performance liquid chromatography analysis of perampanel and stiripentol in mouse matrices

We report a high-performance liquid chromatography method development able to simultaneously determine perampanel and stiripentol, two third-generation antiepileptics whose therapeutic spectrum can potentially be extended, in several mouse matrices. A salting-out assisted liquid-liquid extraction optimized by a design of experiments approach was adopted for sample preparations. Isopropanol and magnesium sulfate were the extraction solvent and salting-out agent, respectively. Both drugs and internal standard (terbinafine) were separated using a LiChroCART® Purospher Star column (C18 , 55×4mm; 3μm) isocratically pumped with mobile phase [1% triethylamine in water (pH 2.5) and acetonitrile (53:47, v/v)] at 1mL/min. Stiripentol and terbinafine were detected by fluorescence at 254/372nm and perampanel at 275/430nm. Good linearity was demonstrated for perampanel at 1-500ng/mL range in brain, 2-2000ng/mL in liver and 1-2000ng/mL in plasma and kidney (r2 ≥0.9922), and for stiripentol between 10 and 2000ng/mL in brain and 10 and 20000ng/mL in the remaining matrices (r2 ≥0.9917). Precision (CV ≤15%) and accuracy (bias ±15%) were also verified, with obtained recovery values consistent with those predicted by the experimental design. This method was applied in preliminary pharmacokinetic studies to quantify perampanel or stiripentol after oral administration to mice, showing to be a promising bioanalytical tool to support future nonclinical in vivo pharmacokinetic studies.

Characteristics of a novel on-line micro pressurized liquid extraction method

A novel on-line micro pressurized liquid extraction (μPLE) method is introduced, which directly interfaces miniaturized solid sample preparation with HPLC for fast analysis. The technique employs rapid heating to remove analytes from 5–10 mg samples in typically 20–40 s using only about 300 μL of solvent. The resulting extract is then internally transferred to an HPLC injector for chromatographic analysis. Results show that good analyte recoveries can be achieved, similar to conventional PLE and off-line μPLE approaches, without manual sample handling. For example, 103% ± 3% (n = 4) of the acetylsalicylic acid present in pharmaceutical tablets was extracted into methanol after 20 s at 180 °C. Further, 105% ± 9% (n = 4) of the caffeine present in a green tea sample was extracted into methanol after 40 s at 275 °C. Typical time to analysis was about 95 s total for most samples, and solvents could also be easily alternated during trials to increase extract selectivity. The on-line μPLE system was applied to the extraction of model PAHs from a biochar matrix and was found to extract 97% ± 5% (n = 4) of anthracene present in the sample after a 30 s static and 60 s dynamic extraction at 220 °C. This yield is much better than results obtained by previous approaches and is attributed to the small size, high temperature, low thermal mass, and dynamic flow of the system. Findings indicate that the on-line μPLE system can greatly assist in such extractions and provide a useful method for rapidly preparing solid samples for analysis using little solvent.

Salting-out Assisted Liquid–Liquid Extraction for Analysis of Caffeine and Nicotinic Acid in Coffee by HPLC–UV/Vis Detector

A salting-out assisted liquid–liquid extraction method followed by high performance liquid chromatography with ultraviolet–visible detector (SALLE-HPLC–UV/Vis) has been proposed for determination of caffeine and nicotinic acid in raw and roasted coffee samples. Various parameters affecting chromatographic separations including mobile phase composition, injection volume, flow rate and column temperature were studied. Experimental parameters affecting the extraction efficiency of SALLE method such as type and volume of the organic solvent, type and amount of salt, pH of the sample, and concentration of the ion-pairing reagent were also studied and thereby optimum conditions were established. The calibration curves which were constructed at five different concentration levels using the optimum conditions exhibited good linearity, with the coefficient of determination (R2) 0.999 and 0.995 for caffeine and nicotinic acid, respectively. The limits of detection (LOD) and quantification (LOQ) which were determined at 3 and 10 times signal-to-noise ratio were 0.05 and 0.13 mg/L for nicotinic acid and 0.20 and 0.63 mg/L for caffeine, respectively. Intra- and inter-day precision studies were demonstrated satisfactory precision with RSD values below 10. Relative recoveries were also studied, and their results were ranging from 82–122% for both raw and roasted coffee samples. The findings demonstrated that the proposed method could be used as an effective and best alternative for the determination of caffeine and nicotinic acid in raw and roasted coffee samples. • SALLE was proposed for extraction caffeine and NA from raw and roasted coffee samples. • HPLC-UV/Vis was used for separation and determination of the target analytes. • The method has exhibited satisfactory analytical performance characteristics and good selectivity for both analytes. • The method uses classical laboratory apparatuses and small volume of less toxic organic solvent. • Compared to the other methods, the proposed method has similar or better LOD and LOQ than the earlier reported methods.

Processing and recycling of iron-bearing copper–nickel production waste

The importance of production waste recycling toward sustainable development of the society is defined. The world’s experience in processing and reusing of metallurgical waste from nonferrous metallurgy works are briefly described. Examples of the use of slag and cake in the construction industry are presented, and a number of technologies for the extraction of nonferrous metals and iron from them are described. To organize efficient utilization of waste slag from Kola MMC, a mixed processing method has been developed based on their sulfuric acid leaching with 5-10% sulfuric acid, transferring most of silica into the solution in the form of silicic acid and concentrating the bulk of nickel and all copper in an insoluble residue, followed by flotation of nonferrous metal sulfides, providing flotation concentrates containing more than 4.5% copper and nickel. Processing of the leaching solution produces mesoporous silica with a specific surface area of 700-800 m2/g, which is used as an active additive in cement. The possibility of hydrometallurgical processing of afterburning products after carbonyl nickel decomposition using hydrochloric acid solutions and liquid extraction method for separating nickel and iron by organic reagents to obtain pure solutions of ferric chloride is demonstrated. A scheme is proposed for the joint processing of solutions from leaching of ferruginous cakes and residues of carbonyl nickel afterburning, as well as nickel raffinates of cobalt production of Kola MMC, which ensures production of commercial ferric chloride. To reduce the volume of dumped iron cakes, the technology and regulation are developed for the extraction of iron(III) from concentrated nickel solutions using high molecular weight aliphatic ketones and their mixtures with fatty alcohols instead of its hydrolytic precipitation.The authors appreciate participation of Leading Researcher, Candidate of Geological and Mineralogical Sciences Yu. N. Neradovskiy and Researcher E. V. Chernousenko from the Tananaev Institute of Chemistry and Technology of Rare Elements and Minerals, Kola Science Center, Russian Academy of Sciences in these studies.

Simultaneous Analysis of Seven Neonicotinoids in Commercial Milk Samples Using an UHPLC-MS/MS Method

A liquid–liquid extraction and ultra high-performance liquid chromatography tandem mass spectrometry (UHPLC–MS/MS) method was developed for simultaneous analysis of the residues of seven neonicotinoid insecticides (NEOs), namely acetamiprid, clothianidin, dinotefuran, imidacloprid, thiacloprid, thiamethoxam, and nitenpyram, in commercial milk samples. The method had a good linearity (R2 > 0.992) and a limit of detection range of 0.004–0.15 μg/kg. The average recovery range was 89–119% with an intraday precision of 1.4–10.3% at spiking levels of 8, 12, and 16 μg/kg. The validated method was employed for routine analysis of the aforementioned seven NEOs in commercial milk samples obtained randomly from a supermarket in Miaoli (Taiwan). The detected thiamethoxam and clothianidin levels were 3.4 and 80 μg/kg, respectively.

Production routes to bio-acetic acid: life cycle assessment

BackgroundSimilar to biofuels, numerous chemicals produced from petroleum resources can also be made from biomass. In this research we investigate cradle to biorefinery exit gate life cycle impacts of producing acetic acid from poplar biomass using a bioconversion process. A key step in developing acetic acid for commercial markets is producing a product with 99.8% purity. This process has been shown to be potentially energy intensive and in this work two distillation and liquid–liquid extraction methods are evaluated to produce glacial bio-acetic acid. Method one uses ethyl acetate for extraction. Method two uses alamine and diisobutyl ketone. Additionally two different options for meeting energy demands at the biorefinery are modeled. Option one involves burning lignin and natural gas onsite to meet heat/steam and electricity demands. Option two uses only natural gas onsite to meet heat/steam demands, purchases electricity from the grid to meet biorefinery needs, and sells lignin from the poplar biomass as a co-product to a coal burning power plant to be co-fired with coal. System expansion is used to account for by-products and co-products for the main life cycle assessment. Allocation assessments are also performed to compare the life cycle tradeoffs of using system expansion, mass allocation, or economic allocation for bio-acetic acid production. Finally, a sensitivity analysis is conducted to determine potential effects of a decrease in the fermentation of glucose to acetic acid.ResultsGlobal warming potential (GWP) and fossil fuel use (FFU) for ethyl acetate extraction range from 1000–2500 kg CO2 eq. and 32–56 GJ per tonne of acetic acid, respectively. Alamine and diisobutyl ketone extraction method GWP and FFU ranges from −370–180 kg CO2 eq. and 15−25 GJ per tonne of acetic acid, respectively.ConclusionsOverall the alamine/diisobutyl ketone extraction method results in lower GWP and FFU values compared to the ethyl acetate extraction method. Only the alamine/diisobutyl extraction method finds GWP and FFU values lower than those of petroleum based acetic acid. For both extraction methods, exporting lignin as a co-product produced larger GWPs and FFU values compared to burning the lignin at the biorefinery.

Endogenous 1-H-Pyrrole-2,3,5-Tricarboxylic Acid (PTCA) in Hair and Its Forensic Applications: A Pilot Study on a Wide Multi-Ethnic Population.

Over the years, several studies have shown that many factors are likely to affect the results of forensic hair analyses and complicate their interpretation. Among these factors, one of the major drawbacks in hair analysis is the affectability of deposited xenobiotics by cosmetic treatments, which could be eventually used to adulterate the sample. It is well known that some cosmetic treatments containing hydrogen peroxide, such as permanent dyeing or bleaching, lead to the formation of 1-H-pyrrole-2,3,5-tricarboxylic acid (PTCA), a melanin degradation product. Considering that PTCA is also an endogenous compound, spontaneously formed by natural oxidation of melanin, its only detection in hair is not enough to confirm a cosmetic oxidative treatment. For this reason, the aim of the present work was to develop and validate a reliable liquid-liquid extraction method in ultra-high-performance liquid chromatographic-tandem mass spectrometry for the determination of endogenous PTCA in hair from a wide multi-ethnic population (African, Arab, Asian-Pacific, Caucasian, Hispanic and Indian). According to previous studies, untreated hair samples showed a PTCA content of 8.54 ± 5.72 ng/mg (mean ± standard deviation [SD]), ranging between 0.44 and 23.7 ng/mg; after in vitro cosmetic bleaching, PTCA increased to 16.8 ± 6.95 ng/mg (range: 4.16-32.3 ng/mg). Comparing baseline PTCA levels of each subgroup with the others, we could not observe any statistically significant difference, except for Caucasians (P < 0.05), wherein the concentrations were lower. Further studies and a wider sampling are necessary to elucidate the role of PTCA as diagnostic marker of cosmetic hair treatment in forensic field.

Simultaneous determination of VD2, VD3, 25(OH) D2, and 25(OH) D3 in human plasma using electrospray LC-MS/MS as well as its application to evaluate VD plasma levels in depressive, schizophrenic patients and healthy individuals.

Vitamin D measurements in biological fluids by liquid chromatography-tandem mass spectrometry (LC-MS/MS) have been widely used but remain challenging at very low concentration levels. Rapid, high recovery, sensitive and reliable measurements of vitamin D, as well as its primary metabolites using LC-MS/MS are urgently needed for a routine clinical laboratory. Herein, we reported a novel electrospray LC-MS/MS method for determining vitamin D and its primary metabolites using the supported liquid extraction method to achieve higher recoveries, with optimized pH values to achieve optimal derivatization efficiency for higher sensitivity and selected chromatographic conditions to shorten the separation time. The method has been validated with respect to selectivity, recovery, matrix effects, accuracy and precision, stabilities, carryover and dilution effects. The method has been successfully applied to quantify the VD plasma concentrations of depressive, schizophrenic patients and healthy individuals. The result showed that there were significant differences in plasma VD levels between mental disorder patients with healthy individuals, and the total VD levels in mental disorder patients were much higher than healthy individuals, which might require larger clinical samples for validation.

Enantiomeric separation and quantification of R/S-amphetamine in serum using semi-automated liquid-liquid extraction and ultra-high performance supercritical fluid chromatography-tandem mass spectrometry.

The amphetamine molecule contains a chiral center and its enantiomers exhibit differences in pharmacological effects, with the S-enantiomer mediating most of the central nervous system stimulating activity. The majority of prescribed amphetamine consists of the pure S-enantiomer, but therapeutic formulations containing the R-enantiomer in various proportions are also available. Illegal amphetamine remains available mainly as a racemic mixture of the R- and S-enantiomers. To distinguish between legal and illegal consumption of amphetamine a method for enantiomeric separation and quantification of R/S-amphetamine in serum was developed and validated using ultra-high performance supercritical fluid chromatography-tandem mass spectrometry (UHPSFC-MS/MS). Sample preparation prior to UHPSFC-MS/MS analysis was performed by a semi-automated liquid-liquid extraction method. The UHPSFC-MS/MS method used a Chiralpak AD-3 column with a mobile phase consisting of CO2 and 0.1% ammonium hydroxide in 2-propanol/methanol (50/50, v/v). The injection volume was 2 μL and run time was 4 minutes. MS/MS detection was performed with positive electrospray ionization and two multiple reaction monitoring transitions (m/z 136.1 > 119.0 and m/z 136.1 > 91.0). The calibration range was 12.5-1,000 nM for each analyte. The between-assay relative standard deviations were in the range of 1.3-3.0%. Recovery was 73% and matrix effects ranged from 95 to 100% when corrected with internal standard. After development and validation, the method has been successfully implemented in our laboratory for both separation and quantification of R/S-amphetamine and has proved to be a reliable and useful tool for distinguishing intake of R- and S-amphetamine in authentic patient samples.

Remediation of PAHs-contaminated water and sand by tropical plant (Eleocharis ochrostachys) through sub-surface flow system

Polycyclic aromatic hydrocarbons (PAHs) removal by the tropical plant, Eleocharis ochrostachys, from contaminated water and sand using sub-surface flow system (SSF) was conducted for 80 days. E. ochrostachys was exposed to various concentrations of diesel (0.5, 1, 2 and 3% v/v). Treatments with and without the plant were conducted to analyse the effect of plants in removing PAHs. A liquid–liquid extraction method was used to extract the PAHs from the wastewater. The PAH removal with plants was significantly better than without plants (p<0.05). At diesel concentrations of 0.5, 1, 2 and 3%, the PAH removal percentages with plants were 89.1, 91.3, 73.0 and 71.6% from water and 95.3, 97.2, 97 and 86.2% from the sand, respectively, while the removals without plants were only 81.8, 81.0, 63 and 63.9% from water and 93.6, 93.9, 95.7 and 81.8% from the sand, respectively. Increasing colony-forming units (CFUs) surrounding the plant roots indicated enhanced growth of rhizobacteria, which could assist the removal of pollutants. Additionally, the gravel layers had removed the total suspended solid (TSS) from 87 to 98%.

Novel bio-analytical technique for estimation of gamma oryzanol in rat plasma and brain homogenate using HPLC

Gamma oryzanol, a component of rice bran oil is used for its anticancer and antihyperlipidemic properties. Bioanalytical method for rat plasma and brain homogenate was developed by HPLC system with a PDA detector in which drug elution was performed using C-18 column (4.6mm×150cm, 5μ) with 1% acetic acid in methanol: acetonitrile (65/35, v/v) as mobile phase at 1.2ml/min flow rate and detected at 326nm wavelength. Liquid liquid extraction method was chosen for extraction of oryzanol from plasma as well as brain homogenate as it provided highest recovery (95% in plasma, 85% in brain homogenate). Various extraction solvents for each body fluid were analysed, out of which highest recovery for plasma (95%), in acetone: IPA (1/1, v/v) and for brain homogenate (85%) in isopropyl alcohol (IPA) was observed. Observed linearity was between 500ng/mL-5000ng/mL. The interday and intraday precision (i.e. %RSD) was less than 10% and accuracy was±5%. Selectivity and matrix effect was checked and found as per USFDA criteria. Plasma samples were found to be stable over the analysis period, HQC samples were stable up to third cycle in freeze and thaw stability while LQC samples were stable over fourth cycle. The method proved to be simple, useful and is appropriate, for preclinical and experimental research.

Surface active ionic liquid‑assisted cloud point extraction method for preconcentration of nickel in environmental samples before its FAAS determination

Green, rapid and modified surface-active ionic liquid assisted cloud point extraction method (SAIL-CPE) was developed to preconcentrate trace levels of nickel Ni(II) ions in environmental samples perior to its detection by FAAS. The proposed method based on utilizing a mixture of a nonionic surfactant (Triton X-114) and a surface-active ionic liquid, 1-hexadecyl-3-methylimidazolium chloride (C16MeImCl), as an extracting phase for Ni(II) ions after the complexation with sunset yellow FCF at pH 6.5. The impact of different analytical parameters on improving the extraction efficiency was invistigated. In the range of 2.0-600 µg L−1, the calibration graph was linear with correlation coefficient of 0.9998. Limit of detection and preconcentration factor were 0.6 and 100. The reliability and precision of the proposed SAIL-CPE system as the relative standard deviation (RSD %) in the presence and absence of SAIL were examined by applying ten replicate determinations of 300 µg L-1 of Ni(II), and RSD % of the recoveries were found to be 1.40 and 2.9%, respectively. The validation of the proposed procedure was verified by test of certified reference materials (TMDA-51.3 fortified water, TMDA-53.3 fortified water and SRM spinach leaves 1570A) applying the standard addition method. Finally, the proposed SAIL-CPE method was developed and applied to preconcentrate and determine of trace levels of Ni(II) ions in real water, food and tobacco samples with satisfactory results.

Recovery of Phytochemicals via Electromagnetic Irradiation (Microwave-Assisted-Extraction): Betalain and Phenolic Compounds in Perspective.

Food colorants processed via agro-industrial wastes are in demand as food waste management becomes vital not only for its health benefits but also for cost reduction through waste valorization. Huge efforts have been made to recover valuable components from food wastes and applied in various fields to prove their versatility rather than for feed ruminant usage only. Betalains and phenolics, antioxidant-rich compounds responsible for host color and so commonly used as natural colorants in food and cosmetic industries, are copiously present in several kinds of fruits and vegetables as well as their wastes. Technological innovation has brought extensive convenient ways of bioactive compounds extraction with many advantages like less use of solvents and energy in a short period of processing time in comparison with the classical solid–liquid extraction methods. Emerging technologies, particularly microwave irradiation, have been amenable to electromagnetic technology for decades. Practically, they have been deployed for functional and supplement food production. In this review, the feasibility of dielectric heating (microwave irradiation) in the extraction of betalain and phenolic compounds mostly from fruit and vegetable wastes was discussed.

FEATURES OF THE COMPOSITION OF FLAVONOIDS IN THE CROWNED SAW-WORT (SERRATULA CORONATA L.S.L.) SIBERIA AND THE FAR EAST OF RUSSIA

One of the common plants in Siberia and the Far East of Russia, but little studied, is the crowned saw-wort (Serratula coronata L.s.l.) of the aster family (Asteraceae). The value of this plant is determined by its high content of phytoecdysteroids and flavonoids. From the aerial part (leaves, stems) of S. coronata L.s.l., growing in Siberia (Altai Region), by liquid extraction methods (70% ethanol) and preparative column chromatography on silica gel in the gradient elution mode with a mixture of solvents (carbon tetrachloride and ethyl alcohol), 2 flavonoids were isolated: quercetin-4'-O-β-D-glucopyranoside, luteolin-4'-O-β-D-glucopyranoside. Identification of the isolated compounds was carried out by UV-, NMR-13C-, 1H, 13C-HMBC-spectroscopy and electrospray mass spectrometry. The reverse-phase high-performance liquid chromatography (RP-HPLC) method was the first to investigate the qualitative composition and quantitative content of individual flavonoids in S. coronata L.s.l. plants growing in Altai and in the Primorsky region of the Russian Federation. The composition of flavonoid glycosides and the distribution of their aglycones in Siberian and Far Eastern plants differ and this can be considered a chemotaxonomic trait of the species S. coronata L.s.l. The spectrophotometry method was used to determine the sum of flavonoids in the aerial organs of crowned saw-wort growing in Altai and Primorsky region. The content of flavonoids in the leaves of the plant (6.7–8.3%) exceeds their content in the stems (0.5–0.9%). Crowned saw-wort sickle is a potential source of biologically active compounds of this class.

Determination of 62 veterinary drugs in feedingstuffs by novel pressurized liquid extraction methods and LC-MS/MS

A fast and simple method for the determination of 62 veterinary drugs in feedingstuffs was developed, optimized, validated, and applied to real samples. Sample preparation was based on a pressurized liquid extraction method using a hard cap coffee machine, which was compared to a commercial pressurized liquid extraction system. Extraction was performed with diatomaceous earth, acetonitrile (20%), and formic acid (0.1%). A central composite design was used to optimize the composition of the extraction solvent. The extracts were analyzed using two chromatographic modes (reversed phase with C18 and HILIC). Analytical limits were set to 25 (limit of detection) and 75 µg kg−1 (limit of quantitation). For banned substances, a salting-out step was included, achieving LOQ lower as 1 µg kg−1 for ractopamine. Other figures of merit such as precision, trueness, decision limit (CCα), method capability (CCβ), matrix effects, stability, recovery, and measurement uncertainty were also reported for analytical validation. The method was successfully applied to hundreds of real samples demonstrating its fitness-for-purpose for the analysis of sulfonamides, tetracyclines, fluoroquinolones, avermectins, quinolones, beta-agonists, beta-lactams, amphenicols, benzimidazoles, coccidiostats, lincosamides, macrolides, nitrofurans, quinoxalines, melamine, and trimethoprim.

Извлечение и разделение кадмия и никеля из водных двухфазных систем методом жидкостной экстракции, соответствующей концепции “зеленая химия”

Extraction of valuable metals from chemical current sources allows not just to solve the problem of their disposal, but also to prevent environmental pollution. This approach is of particular importance in the case of the presence of toxic metals in chemical current sources, such as cadmium. Cadmium is known to have general toxic, mutagenic and teratogenic effects on living organisms. Nickel can cause allergic reactions and have a general toxic effect. According to some reports, nickel has a carcinogenic and mutagenic effect. The aim of the work is to obtain data on the extraction and separation of cadmium and nickel during the disposal of chemical current sources by liquid extraction, depending on the process conditions. The work obtained data on the separation, extraction of cadmium and nickel from Ni–Cd chemical current sources (CСS) using an two-phase aqueous extraction system consisting of polyethylene glycol (PEO-1500), a phase-forming salt of Na2SO4 and water. The extraction behavior of metals and their separation into lower and upper phases using an extractant, potassium iodide, was studied. The maximum recovery of Cd (99.2 ± 1)% and Ni (89.4 ± 1)% is achieved by leaching the batteries with HCl under the following conditions: KI concentration of 3 g/l, dilution coefficient of the CСS solution is 35. The liquid extraction method used in this work has been shown to be effective for the separation of the metals in question and has an advantage in terms of environmental safety. This extraction technique corresponds to the concept of "green chemistry".