Optimization of Extraction Conditions for Flavonoid Composition and Antioxidant Activity of Radix Scutellariae

Microwave, ultrasonic, and reflux extraction were compared to provide an optimized method for flavonoids from Radix Scutellariae including the antioxidant activity of the extracts. The antioxidant activities of the extracts were evaluated by 2,2-diphenyl-1-picrylhydrazyl and oxygen radical absorbance capacity assays. Baicalin, wogonoside, baicalein, wogonin, and oroxylin A were quantified using ultra-high performance liquid chromatography. For microwave extraction, with a ten minutes treatment, the extraction efficiencies of the analytes were higher than treatments by refluxing for 180 minutes and sonication for sixty minutes. In addition, the antioxidant activity of the microwave extracts was slightly higher than the extracts obtained by the other methods. Microwave extraction conditions were further optimized by a single-factor experiment and the optimum conditions were 50 percent ethanol–water (volume by volume), an extraction temperature of 100 degrees celsius, an extraction time of ten minutes, and a sample to solvent ratio of 1:50. This study combines extraction, phytochemistry, and bioactivity to screen the most efficient extraction procedure for flavonoids from Radix Scutellariae.     

Atomic Absorption Spectrometric and Synergistic Spectrophotometric Microdetermination of Hafnium in Alloys and Environmental Samples

Abstract

Hafnium (IV) was selectively extracted from 0.45–0.55 M HC1 media as its chelate with N-p-methoxyphenyl-2-furylacrylo-hydroxamic acid (MFHA) into chloroform. Xylenol orange was added to the extract to form an intensely coloured ternary complex measurable spectrophotometrically at 545 nm (? = 8.3×10⁴1 mol^?1 cm^?1) with a sensitivity better than 0.002 ppm. For atomic absorption spectrometric determination, hafnium was extracted with MFHA into methyl isobutyl ketone and measured with 286.6 nm resonance line in the nitrous oxide-acetylene flame. The methods were applied to the analysis of hafnium in alloys, plant tissues, animal tissues and natural waters. The MFHA-xylenol orange reagent combination was chosen after studying ten hydroxamic acids and five chromogenic reagents.     

Determination of Gold(III) by Simplified Room-Temperature Ionic Liquid Extraction with Flame Atomic Absorption Spectrometry

A new simplified extraction of gold(III) using a room-temperature ionic liquid prior to determination by flame atomic absorption spectrometry has been developed. The extraction method uses 1-butyl-3-methylimidazolium hexafluorophosphate without a chelating agent. The parameters of the extraction system were investigated in detail. Under the optimized conditions, a linear range of 0.19 to 38.20 µg · mL^?1, a limit of detection of 0.072 µg · mL^?1, an enrichment factor of 10.0, and an extraction capacity of 6.6 mg · g^?1 were obtained. The extraction mechanism and the selectivity of 1-butyl-3-methylimidazolium hexafluorophosphate for gold(III) were also investigated. The method was applied for the determination of gold(III) in water samples with satisfactory results.     

n-Octylated Magnetic Nanoparticle-Based Microextraction for the Determination of Organophosphorus Pesticides in Water

A sensitive and simple procedure based on the dispersive solid phase extraction with hydrophobic n-octyl-modified magnetic iron oxide nanoparticles as the sorbent was developed for the determination of ethoprophos, fenchlorphos, parathion methyl, chlorpyrifos, prothiofos, and azinphos methyl in environmental water samples. Dispersive liquid–liquid microextraction was coupled with dispersive solid-phase microextraction to enhance the dispersibility of the selected sorbent and extraction efficiency. The organophosphorus pesticides were detected using gas chromatography with a flame photometric detector. Under optimized conditions, this method achieved low method detection limit (0.02–0.10 microgram per liter), wide linearity (0.5–800 microgram per liter), high enrichment factors (122–143), good correlation coefficients (r = 0.9975–0.9997), and good repeatability (0.2–7.1 percent). This method was also successfully applied to analyze drinking water and surface water with good extraction efficiency (≥82 percent) and high degree of precision (≤5 percent). The results also indicated that the dispersibility of hydrophobic magnetic nanoparticles was enhanced with liquid–liquid microextraction without chemical modification of the magnetic iron oxide nanoparticles.     

Decyl‐perfluorinated magnetic mesoporous microspheres for extraction and analysis perfluorinated compounds in water using ultrahigh‐performance liquid chromatography–mass spectrometry

In this work, the interior‐walls decyl‐perfluorinated functionalized magnetic mesoporous microspheres (F₁₇–Fe₃O₄@mSiO₂) were synthesized for the first time, and applied as adsorbents to extract and concentrate perfluorinated compounds (PFCs) from water samples. The fluorous functionalized interior pore‐walls contributed to the high‐selective preconcentration of PFCs due to fluorous affinity; and abundant silanol groups on the exterior surface of microspheres contributed to the good dispersibility in water sample. Four kinds of PFCs were selected as model analytes, including perfluorooctanoic acid, perfluorononanoic acid, perfluorododecanoic acid, and perfluorooctane sulphonate. In addition, UHPLC‐ESI/MS/MS was introduced to the fast and sensitive detection of the analytes after sample pretreatment. Important parameters of the extraction procedure were optimized, including salinity, eluting solvent, the amount of F₁₇–Fe₃O₄@mSiO₂ microspheres, and extraction time. The optimized procedure took only 10 min to extract analytes with high recoveries and merely 800‐μL acetonitrile to elute analytes from the magnetic adsorbents. Validation experiments showed good linearity (0.994–0.998), precision (2.6–7.6%), high recovery (93.4–105.7%) of the proposed method, and the limits of detection were from 0.008 to 0.125 μg/L. The F₁₇–Fe₃O₄@mSiO₂ magnetic microspheres have the advantages of great dispersibility in aqueous solution, high specificity of extraction, large surface area, and efficient separation ability. The results showed that the proposed method based on F₁₇–Fe₃O₄@mSiO₂ microspheres is a simple, fast, and sensitive tool for the analysis of PFCs in water sample.     

银杏叶中黄酮类化合物的提取、纯化及测定方法的研究进展

对应用于银杏叶中黄酮类化合物的提取方法、纯化方法和测定方法的现状(主要在1999～2011年间发表的文献)及相关的原理和方法的特点作了综述。     

Effect of temperature on the extraction of Pd by liquid tin from molten borosilicate glass containing simulated radwaste

Separation of Pd from borosilicate glass-melt containing simulated high level radioactive waste (Pd, Mo, Cs, Sr, Zr, Nd, Ni, Fe) using Sn as the solvent metal was studied on lab scale. The separation of Pd was studied using varying amounts of Sn, and the percentage of extraction of Pd and other elements was investigated by varying the process temperature and the starting material for Pd. The process temperature was observed to have a profound influence on the separation of Pd from the glass melt to the metallic tin phase. The % extraction of Pd was found to be less for the batches heat-treated at temperatures below 900 °C. The decrease in the % extraction was due to the entrainment of Pd in the glass phase for the samples heat-treated at low temperatures. The entrainment of Pd leads to the formation of Pd-rose like structures in the glass phase as observed by SEM and EDAX. Similarly, Mo, Fe and Na also formed separate phases inside glass matrix when the samples were heated below 900 °C. However, entrainment was not seen when the samples were heat-treated above 1050 °C in Ar. At 1200 °C, a recovery of about 99% of Pd was obtained. The formation of a PdSn₄ type intermetallic phase was noticed in tin metallic phase. The extraction behavior of Pd in borosilicate glass melt was also studied by using Pd(NO₃)₂ instead of Pd powder as staring material, and the results showed that the process temperature is the key determinant of the extraction behavior of Pd.     

Optimizing conditions for the extraction of catechins from green tea using hot water

Six different factors involved in the extraction of catechins from green tea using water were examined for their impact on the yield of catechins and on the efficiency of water use. The best temperature and time combination for catechin extraction was at 80°C for 30 min. The yield of catechins was also optimal with a tea particle size of 1 mm, a brewing solution pH <6 and a tea‐to‐water ratio at 50:1 (mL/g). In terms of efficient use of water in a single extraction, a water‐to‐tea ratio of 20:1 (mL/g) gave the best results; 2.5 times less water was used per gram of green tea. At the water‐to‐tea ratio of 20:1 mL/g, the highest yield of catechins per gram of green tea was achieved by extracting the same sample of green tea twice. However, for the most efficient use of water, the best extraction was found to be once at a water‐to‐tea ratio of 12:1 (mL/g) and once at a water‐to‐tea ratio of 8:1 (mL/g). Therefore, all six of the factors investigated had an impact on the yield of catechins extracted from green tea using water and two had an impact on the efficiency of water use.     

Polynomial-based non-uniform interpolatory subdivision with features control

Starting from a well-known construction of polynomial-based interpolatory 4-point schemes, in this paper we present an original affine combination of quadratic polynomial samples that leads to a non-uniform 4-point scheme with edge parameters. This blending-type formulation is then further generalized to provide a powerful subdivision algorithm that combines the fairing curve of a non-uniform refinement with the advantages of a shape-controlled interpolation method and an arbitrary point insertion rule. The result is a non-uniform interpolatory 4-point scheme that is unique in combining a number of distinctive properties. In fact it generates visually-pleasing limit curves where special features ranging from cusps and flat edges to point/edge tension effects may be included without creating undesired undulations. Moreover such a scheme is capable of inserting new points at any positions of existing intervals, so that the most convenient parameter values may be chosen as well as the intervals for insertion.Such a fully flexible curve scheme is a fundamental step towards the construction of high-quality interpolatory subdivision surfaces with features control.     

The effect of adding a standard on the result of determination of polychlorinated biphenyls in bottom sediment samples

Bottom sediments are a very important component of aquatic ecosystems. The sediment matrix is highly diverse and heterogeneous; in consequence, compounds entering the aquatic environment from different sources are considerably enriched at its surface. Bottom sediments are regarded as natural sorbents, since they accumulate many harmful substances, such as heavy metals and stable organic contaminants.Extraction is a key stage in every analytical procedure. It is during this stage that standards are added to samples. Standards are necessary not only for estimating analyte yields but also for validating the whole procedure. The question of the addition of standard substances to sediment samples has not been widely addressed in the subject literature, and yet it is of fundamental importance as regards obtaining reliable results of determinations.This paper describes the results of a study on the effect of standard addition techniques on the results of determination of polychlorinated biphenyls in sediment samples (certified reference material: METRANAL™2—river sediment).