• Analytical Science and Technology
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• v.9 no.3
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• pp.221-234
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• 1996

Basic studies for the effective extraction of dibenzylammonium dibenzyldithiocarbamate(DBADBDC) complexes of Ag(I), Pd(II), Au(III) and Pt(IV) into chloroform have been conducted. The effects of pH on the extraction of ligand itself and metal cemplexes showed that DBADBDC itself was uniformly extracted in the pH range of 2~9 and metal complexes were effectively extracted at the pH range as follows. That is, Ag(I) : in an acidic aqua medium, Pd(II) : > 4, Au(III) : wide range, and Pt(IV) : > 3. The distribution ratio and extractabilities were obtained from the partition and extraction equilibria of metal-DBDC complexes between aqueous solution and chloroform. Ag(I) : log D=4.226 : E(%)=99.9% in the aqueous solution of pH 0, Pd(II) : log D=1.804 : E(%)=98.5% at pH 4~7, Au(III) : log D=3.755 : E(%)=99.9% at pH 2~10, and Pt(IV) : log D=0.165 : E(%)=57.2% at pH 8.0. And also mole ratio of metal ion to ligand in complexes were determined by mole ratio method : 1 : 1 for Ag(I) and 1 : 2 for Pd(II), Au(III) and Pt(IV). $Cl^-$ was included as a coordination species in complexes of Au(III) and Pt(IV). Besides, extraction mechanisms of compleses sere examined in the presence of chloride ion in an aquous solution, and extraction reactions and estraction constants could be proposed and calculated, respectively.

• Applied Biological Chemistry
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• v.4
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• pp.23-28
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• 1963

Various species of the genus Capsicum contain in their fruits an intensively sharp and pungent substance, Capsaicin, which was first isolated in an almost pure state by Thresh. Containing the pungent principle, Capsicums are used extensively in food as a spice and in medicine as a rubefacient and carminative. Numerous methods have been proposed for the isolation, the chemical structure and the quantitative determination of Capsaicin. Modifying the several methods described before, the Capsaicin contents in various species of the genus Capsicum were determined as follows. (1) The isolation of pure Capsaicin was the essential first step for the determination of Capsaicin contents. Powdered cayenne pepper was extracted with acetone. By the method of ether alkali partition extraction slightly modified at this laboratory and by the recrystallization with light petroleum ether that was repeated ten times, the pure crystalline Capsaicin was obtained. Using this Capsaicin, the standard absorption curve was drawn with Beckman spectrophotometer model DU for the quantitative determination of Capsaicin. 92) The powdered sample was extracted in a Soxhlet extractor with ether-acetone solvent system(3:1) for 25 hours. Capsaicin in this ether-acetone extracts was efficiently separated in a pure state by paper partition chromatography using 58% methanol solution as developing agent. It was found that 58% methanol was one of the most valuable solvent to separate Capsaicin from impurities such as sterols, fatty acids, waxes and carotenoid pigments. (3) The colorimetric method modifying the Schulte-Kruger's method which consists of measuring the red color produced with diazobenzenesulphonic acid was used. Capsaicin in various species of the genus Capsicum was determined quantitatively with use of Beckman spectrophotometer model DU at $480\;m{\mu}$.

• Journal of the Korean Chemical Society
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• v.36 no.1
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• pp.66-74
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• 1992

A method for the multiresidual simultaneous analysis of 11 thiocarbamates was studied using HPLC. Thiocarbamate in Chinese cabbage was analyzed in the order of extraction, partition, and cleanup in their optimum condition. Acetone was chosen as an extracting solvent. As a partitioning solvent, the mixture of 50% methylene chloride and petroleum ether containing extremely small water content showed good recoveries of thiocarbamate from the water layer. Partition efficiency was affected by pH of the water layer; it remained almost constant under the acidic and neutral condition while decreasing under the basic condition. The comparison done in cleanup step showed that the column chromatographic method is superior to the treatment of coagulating reagent. As an absorbent, the mixture of charcoal, magnesia, and celite with the ratio of 1 : 2 : 4 gave better recoveries and also effectively removed chlorophyll. Over the total procedure, the average recoveries for thiocarbamates in Chinese cabbage were 91% at about 2 ppm fortification level within the relative standard deviation of 8%, and the minimum detection limit (MDL) was 2.2${\sim}$9.3 ng.

• Korean Journal of Food Science and Technology
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• v.28 no.1
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• pp.77-82
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• 1996

Antioxidative activity of the extract from Caesalpinia sappan L. by various solvent was compared with several commercial antioxidants, using the Rancimat method. AI (antioxidative index; induction period of oil containing extract/induction period of control oil) of all extracts were higher than commercial antioxidants, such as BHA, ${\delta}-tocopherol$ and ascorbic acid. The ethanol extract was fractionated by liquid liquid extraction. Ethyl acetate fraction showed higher AI than the whole crude extract. When comparing POV and TBA value of palm oil and lard containing different level of each fraction, the oxidative stability of ethyl acetate fraction at 200 ppm level on palm oil and lard were similar to that of BHT at 200 ppm level, and better than BHA, ${\delta}-tocopherol$ and control.

• Journal of the Korean Society of Food Science and Nutrition
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• v.44 no.5
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• pp.775-783
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• 2015

This study was carried out to investigate the physicochemical properties and volatile ingredients of Jeju Apple mango subjected to different extraction methods and GC/MS. The crude protein, fat, and ash contents were $0.22{\pm}0.01$, $0.09{\pm}0.00$, and $0.27{\pm}0.02%$, respectively, and contents of free sugar increased in the order of sucrose, fructose, and glucose, whereas maltose, lactose, and galactose were not detected. The numbers of volatile flavor compounds obtained by the SE (solvent extraction), SDE (simultaneous steam distillation extraction), and SPME (solid-phase micro-extraction) methods were 51, 59, and 71, respectively. The percentages of extracted volatile flavor compounds in mango were 11.44, 15.68, and 73.54% by the SE, SDE, and SPME methods, respectively. The most abundant compounds found in Jeju Apple mango were terpenes and their derivatives, which accounted for 44.49~94.57% of total volatiles obtained. SPME method was considered to be the most effective extraction method in terms of the numbers of detected compounds and their amounts. ${\delta}$-3-Carene was identified as the dominant compound in mango, whereas ${\alpha}$-phellandrene, ${\gamma}$-terpinene, trans-${\beta}$-ocimene, ${\alpha}$-terpinolene, limonene, ${\alpha}$-pinene, and furaneol were the next important compounds.

• Bulletin of the Korean Chemical Society
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• v.32 no.5
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• pp.1547-1553
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• 2011

An effective analytical method of gas chromatography/mass spectrometry (GC/MS) was developed for the rapid determination of essential oils in the crude extract of Acorus species (Acorus gramineus, Acorus tatarinowii, and Acorus calamus). Major phenypropanoids (${\beta}$,${\alpha}$-asarone isomers, euasarone, and methyleugenol) and ${\beta}$-caryophyllene in Acorus species were used as marker compounds and determined for the quality control of herbal medicines. To extract marker compounds, various extraction techniques such as solvent immersion, mechanical shaking, and sonication were compared, and the greatest efficiency was observed with sonication extraction using petroleum ether. The dynamic range of the GC/MS method depended on the specific analyte; acceptable quantification was obtained between 10 and 2000 ${\mu}g/mL$ for ${\beta}$-asarone, 10 and 500 ${\mu}g/mL$ for ${\alpha}$-asarone, 10 and 200 ${\mu}g/mL$ for methyleugenol, and between 5 and 100 ${\mu}g/mL$ for ${\beta}$-caryophyllene. The method was deemed satisfactory by inter- and intra-day validation and exhibited both high accuracy and precision, with a relative standard deviation < 10%. Overall limits of detection were approximately 0.34-0.83 ${\mu}g/mL$, with a standard deviation (${\sigma}$)-to-calibration slope (s) ratio (${\sigma}$/s) of 3. The limit of quantitation in our experiments was approximately 1.13-3.20 ${\mu}g/mL$ at a ${\sigma}$/s of 10. On the basement of method validation, 20 samples of Acorus species collected from markets in Korea were monitored for the quality control. In addition, principal component analysis (PCA) and hierarchical cluster analysis (HCA) were performed on the analytical data of 20 different Acorus species samples in order to classify samples that were collected from different regions.

• Nuclear Engineering and Technology
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• v.48 no.3
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• pp.727-732
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• 2016

A simple and rapid spectrophotometric method has been developed to enable the determination of plutonium concentration in an irradiated fuel solution in the presence of all fission products. An excess of ceric ammonium nitrate solution was employed to oxidize all the valence states of plutonium to +6 oxidation state. Interference due to the presence of fission products such as ruthenium and zirconium, and corrosion products such as iron in the envisaged concentration range, as in the irradiated fuel solution, was studied in the determination of plutonium concentration by the direct spectrophotometric method. The stability of plutonium in +6 oxidation state was monitored under experimental conditions as a function of time. Results obtained are reproducible, and this method is applicable to radioactive samples resulting before the solvent extraction process during the reprocessing of fast reactor spent fuel. An analysis of the concentration of plutonium shows a relative standard deviation of <1.2% in standard as well as in simulated conditions. This reflects the fast reactor fuel composition with respect to uranium, plutonium, fission products such as ruthenium and zirconium, and corrosion products such as iron.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.19 no.5
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• pp.436-445
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• 1986

As the second part of the studies on the utilization of polyunsaturated lipids in sardine oil as nutritional or medical supplement, the conditions of lipid extration and concentration, refining, and storage stability of EPA-condensed sardine oil were investigated. In extraction of lipids, solvent ratios of chloroform-methanol mixture(2:1 v/v) affected the final content of unsaturated lipid in extracted oil and recovery. Stepwise solvent fractionation method at various low temperatures was effective to concentrate polyenoic acids like EPA and DHA when acetone or acetone-methanol mixture, added in the ratio of 1:5 (v/v) was applied step by step to different temperatures at 0 to $-35^{\circ}C$. Addition of 1 to $5\%$ (v/v) of water to acetone was also benefit to raise EPA content but that resulted in reducing the yield of condensed oil from $65\%\;to\;28\%$. Concentration rate of polyenoic acids by solvent fractionation in lipid-actone solution (1:5, v/v) at 0 to $-30^{\circ}C$ seemed limited to $5{\sim}8\%$ in fatty acid composition depending on the initial content of those polyenoic acids in the sardine oil. During the extraction, concentration, and alkaline treatment, oxidation was rapidly induced but oxidation products could be thoroughly removed on the process of deceleration and peroxide elimination. To stabilize the reactive polyenoic acid condensed oil during the storage, stuffing nitrogen gas was essential to expel dissolved oxygen in oil or to seal the oil from open air, and the addition of antioxidative agents as BHA and tocopherols were greatly helpful to extend the storage life.

• Analytical Science and Technology
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• v.15 no.2
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• pp.127-134
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• 2002

Analytical method to determine rare earth elements which were extracted to organic phase by inductively coupled plasma mass spectrometry(ICP-MS) was investigated. Organic phase which had extracted rare earth elements was directly aspirated into ICP-MS by ultrasonic nebulizer(USN) in order to reduce solvent load to the plasma. Then, the count rate increased when MIBK(methyl isobutyl ketone) was added to EtOH(ethanol) but decreased when 0.03 M HEH(2-ethylhexyl-2-ethylhexyl phosphonic acid, $P_{507}$, PC88A) was added to solvent which mixed MIBK with EtOH. The optimal temperatures of desolvation system were -10 $^{\circ}C$ for the condenser and 150 $^{\circ}C$ for the heating tube. The optimal nebulizer flow rate which gave maximum count rate and minimum reflect power was 0.7 L/min. The optimal pH and extraction time were 4.3 and 10 min for MIBK-0.03 M HEH system. Detection limits which were obtained through calibration curves at the range of 0.2 ${\sim}$ 20 ng/mL were 0.02 ${\sim}$ 0.05 ng/mL under the optimal experimental conditions.

• Journal of Korean Society of Environmental Engineers
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• v.37 no.5
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• pp.262-268
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• 2015

This study established an analytical method to simultaneously determine six organophosphorous pesticides [methyldemetone-S, diazinon, fenitrothion, parathion, phentoate, and O-ethyl O-(4-nitrophenyl) phenylphosphonothioate (EPN)] and carbaryl in water using a gas chromatography/mass spectrometry (GC/MS) system coupled with on-line micro extraction by packed sorbent (MEPS) and programmed temperature vaporizer (PTV) injector. Polystyrene divinylbenzene (PDVB) was used as a sorbent of MEPS. The effects of elution solvents, pH, elution volume and draw-eject cycles of samples on sample pretreatment process were investigated. Also, quality assurance and quality control (QA/QC) and the recovery of the pesticides in environmental samples were evaluated. The elution was performed using $30{\mu}L$ of a mixed solvent (acetone : dichloromethane = 80 : 20 (v/v)). Sample pretreatment processes were optimized with seven cycles of draw-eject of sample (1 mL) spiking an internal standard and sulfuric acid. At lower pH, the analytical sensitivity of diazinon decreased, but that of carbaryl increased. The method detection limit and the limit of quantification for this method were 0.02~0.18 and $0.08{\sim}0.59{\mu}g/L$, respectively. The method precision and accuracy were 1.5~11.5% and 83.3~129.8%, respectively, at concentrations of $0.5{\sim}5.0{\mu}g/L$. The recovery rates for all the pesticides except carbaryl in various environmental samples ranged 75.7~129.3%. The recovery rate of carbaryl in effluent sample was over 200% whereas carbaryl in drinking water, groundwater, and river water were in the acceptable range.