• Analytical Science and Technology
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• v.9 no.4
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• pp.336-344
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• 1996

The extraction of trace cobalt, copper, nickel, cadmium, lead and zinc in urine samples of organic and alkali metal matrix into chloroform by the complex with a dithizone was studied for graphite furnace AAS determination. Various experimental conditions such as the pretreatment of urine, the pH of sample solution, and dithizone concentration in a solvent were optimized for the effective extraction, and some essential conditions were also studied for the back-extraction and digestion as well. All organic materials in 100 mL urine were destructed by the digestion with conc. $HNO_3$ 30 mL and 30% $H_2O_2$ 50 mL. Here, $H_2O_2$ was added dropwise with each 5.0 mL, serially. Analytes were extracted into 15.0 mL chloroform of 0.1% dithizone from the digested urine at pH 8.0 by shaking for 90 minutes. The pH was adjusted with a commercial buffer solution. Among analytes, cadmium, lead and zinc were back-extracted to 10.00 mL of 0.2 M $HNO_3$ from the solvent for the determination, and after the organic solvent was evaporated, others were dissolved with $HNO_3-H_2O_2$ and diluted to 10.00 mL with a deionized water. Synthetic digested urines were used to obtain optimum conditions and to plot calibration-eurves. Average recoveries of 77 to 109% for each element were obtained in sample solutions in which given amounts of analytes were added, and detection limits were Cd 0.09, Pb 0.59, Zn 0.18, Co 0.24, Cu 1.3 and Ni 1.7 ng/mL, respectively. It was concluded that this method could be applied for the determination of heavy elements in urine samples without any interferences of organic materials and major alkaline elements.

• Analytical Science and Technology
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• v.8 no.3
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• pp.321-334
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• 1995

Basic studies for the effective extraction of ammonium pyrrolidine dithiocarbamate(APDC) complexes of Co(II), Ni(II) and Cu(II) into a solvent have been performed. The maximum distribution ratio was appeared (log D=1.3543) at pH 2.0 and the partition coefficient was 2.489 in the extraction of $4{\times}10^{-5}M$ APDC itself into chloroform. From the UV/visible spectra of metal-chelates in aqueous and organic solutions, the pH to form stable 1:2 metal-ligand complexes were Co(II):5.0, Ni(II):8.0 and Cu(II):8.0, respectively and only 1 minute was enough to be partitioned into the chloroform. Besides, the partition and extraction equilibria of the complexes were investigated by back-extracting $10.0{\mu}g/ml$ metal-chelates from the solvent into an aqueous solution beacuse of their slight solubilities in the aqueous solution. The distribution coefficients and extractabilities were as follows : at pH 6.5~8.5 of the aqueous solution, log D=2.834 : E(%)=99.9% for $Co(PDC)_2$, at pH 11, log D=5.699 E%=100 for $Ni( PDC)_2$, and at pH 6.0, log D=2.025 : E(%)=99.1% for $Cu(PDC)_2$. And the extraction and formation constants were log $K_{ex}=9.671$ : log ${\beta}_2=6.938$ for $Co(PDC)_2$, log $K_{ex}=9.646$ : log ${\beta}_2=7.071$ for $Ni( PDC)_2$, and log $K_{ex}=9.074$ : log ${\beta}_2=7.049$ for $Cu(PDC)_2$, respectively. From these results, an optimum extraction procedure can be constructed for the separative concentration of trace metallic ions, and the quantitative determination of them in advanced materials and environmental samples will be expected without any influence of sample matrixes.

• Journal of the Korean Society of Food Science and Nutrition
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• v.40 no.5
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• pp.665-672
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• 2011

We evaluated the effects of organic Ca supplements chelated with milk protein (CaMP) in ovariectomized osteoporotic rats. Eight week-old Sprague-Dawley female rats were ovariectomized and fed a low $CaCO_3$ diet (0.1%) for 4 weeks to create an osteoporotic model. At that point, L4-$CaCO_3$ rats were sacrificed and the rest of the rats were divided into 4 groups, each of which was fed an experimental diet for 4 weeks: low-$CaCO_3$ (0.1%; L8-$CaCO_3$) and CaMP at 3 Ca levels: low (0.1%; L8-CaMP), normal (0.5%; N8-CaMP), and high (1.5%; H8-CaMP). Daily weight gain, serum ALP, weight and breaking force of femurs, Ca content of the lumbar, and Ca absorption were measured. Daily weight gain increased in the N8-CaMP and H8-CaMP groups compared to the low Ca groups. The ALP activity in the CaMP-fed rats was significantly lower than in the $CaCO_3$-fed rats. Both breaking force and femur weight were higher in the N8-CaMP and H8-CaMP groups compared to the L8-$CaCO_3$ group. Ca content of the lumbar increased dose-dependently with Ca intake levels of CaMP. Ca absorption rates of the CaMP-fed rats increased more than that of the rats fed low Ca levels of $CaCO_3$. These results demonstrate that the CaMP supplement had positive effects on bone metabolism and Ca bioavailability in ovariectomized osteoporotic rats. Therefore, CaMP may be recommended as a useful Ca supplement to prevent bone loss in osteoporosis.

• Journal of the Korean Chemical Society
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• v.38 no.12
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• pp.898-907
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• 1994

The solvent extraction of an inorganic trace mercury in sea water samples was studied using zinc diethyldithiocabamate $Zn(DDC)_2$ as chelating agent. The $Zn(DDC)_2$ which maintained the stability of DDC- in the acidic aqueous solution in the course of extraction was synthesized from NaDDC and $ZnSO_4$ in this laboratory. The trace of mercury(Ⅱ) was extracted at pH 3.0 from 100 ml of sea water into 10ml of chloroform containing 0.05 M $Zn(DDC)_2$ by shaking for 5 minutes. And from the organic phase, the $Hg(DDC)_2$ was back-extracted into 10ml of 1 to 1 mixed acid of each 3% (v/v) nitric acid and hydrochloric acid by shaking for 25 minutes. The mercury back-extracted was determined by a cold vapor atomic absorption spectrophotometry. The trace mercury(Ⅱ) was so successfully extracted that this procedure could be applied to its determination in the sea water. That is, the recoveries of mercury in two kinds of samples into which as given amount of Hg(Ⅱ) was spiked were 90.0% and 93.3%, respectively.

• Journal of Life Science
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• v.18 no.2
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• pp.220-227
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• 2008

To clarify the antioxidation effect of the various solvent fractionation of Tetragonia tetragoniodes which has been known to superior plants for the traditional prevention and treatment of stomach-related diseases, total polyphenol and flavonoid contents, vitamin E content, the elimination activity of a DPPH free radical and superoxide anion, inhibition activity of the superoxide generation, reducing power and metal chelating effects were estimated. The contents of the polyphenol compounds were highest in the DCM and EA fractionation, and the content of flavonoid was high in the order of HX and EA fractionation. The vitamin E content showed high in the order of the HX and DCM fractionation among solvent fractions. $IC_{50}$ for the elimination effect of a DPPH radical were estimated as 554.25 and $394.96{\mu}g/ml$ in the DCM and EA fractions, respectively. These values were higher than that of BHT $784.7{\mu}g/ml$ widely used in antioxidation effect. The inhibition activity of the superoxide generation using the T. tetragoniodes solvent fractions represented the effects similar to that of ${\alpha}$-tocopherol known to prevent the lipoprotein oxidation, but lower consequences than that of the phenol-resins, BHT and BHA, respectively. In the antioxidation activity derived by the reducing capability, the EA fractionation in a 1.5 mg/ml concentration showed higher than that of ${\alpha}$-tocopherol.

• Analytical Science and Technology
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• v.7 no.3
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• pp.361-369
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• 1994

Voltammetric behavior of some light lanthanide ions($La^{3+}$, $Pr^{3+}$, $Nd^{3+}$, $Sm^{3+}$ and $Eu^{3+}$) in acetonitrile(AN) and dimethylformamide(DMF) has been investigated by direct current, differential pulse polarography and cyclic voltammetry. The reduction of $La^{3+}$, $Pr^{3+}$ and $Nd^{3+}$ in 0.1M TEAP proceeded directly to the metallic state through three-electron charge transfer of irreversible process where as $Sm^{3+}$ and $Eu^{3+}$ proceeded by charge transfer of two steps. As the results of the cyclic voltammetric investigation, the first step reduction of $Sm^{3+}$ and $Eu^{3+}$ were a quasireversible reaction, the second step reductions were an irreversible reaction. The cathodic peak currents of the differential pulse polarogram showed adsorptive properties at lower sweep rates and high concentrations of these metal ions. The peak potenital was shifted to a negative petential and the peak current decreased with the increase of percentage of water in AN. On the other hand, the peak potential was shifted to a positive potential and the peak current decreased with an increased percentage of water in DMF.

• Korean Journal of Food Science and Technology
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• v.48 no.6
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• pp.574-581
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• 2016

Glasswort (Salicornia herbacea L.) is an edible halophyte that grows in salt marshes. In the present study, anti- and pro-oxidant activities and cytotoxic properties of glasswort were investigated. Solvent fractions, including fractions of hexane, ethylether (Fr.E), ethylacetate (Fr.EA), butanol and water, were prepared from a 70% methanol extract of glasswort aerial parts. Fr.EA contained the highest levels of total polyphenols and flavonoids, showing the strongest scavenging activities against DPPH and ABTS radicals, and nitrite. In addition Fr.EA showed the most potent cytotoxic effects on HCT-116 colon cancer cells and INT-407 normal intestinal cells, followed by Fr.E. Most fractions also decreased the level of reactive oxygen species in the treated cells, but generated $H_2O_2$ in the medium. The cytotoxic activity of Fr.EA was more pronounced in the presence of ascorbic acid or N-acetylcysteine. These results indicate that the fractions from aerial parts of glasswort exhibit both anti- and pro-oxidant activities, and these activities modulate cytotoxic properties.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.16 no.3
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• pp.216-224
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• 1983

This work was undertaken to obtain some characteristics of proteolytic enzyme of marine gastropods such as sea hare, Aplysia kurodai, top shell, Turbo cornutus, and abalone, Haliotis discus hannai. An influence of pH, temperature and some chemicals on proteolytic activity of the crude enzyme extracted from digestive tract of the samples was taken into account and the stability of the enzyme during the storage at low temperature was also discussed. In comparison of the activities of the crude enzyme from the samples to the optimum conditions, it was characterized that abalone has twice or the more times higher activities than the other two species of the gastropoda in the acid and weak acid region, while, in the alkaline region, sea hare has six or the more times higher acitivities than the other two species. The proteolytic activity was facilitated by $Mn^{2+}$, some reducing agents, EDTA and DTT, and inhibited by $Hg^{2+}$ and SDS, but the other chemicals were not significantly affected to the activity. The low temperature storage of the enzymes of sea hare and top shell at $0^{\circ}C\;or\;-20^{\circ}C$ was not affected to the enzymic activity under the optimum pH condition except in the alkaline region. On the other hand, the low temperature storage was brought about no significant effect on the activity of the enzymes extracted from abalone under the optimum condition of the weak acid region, but apparently influenced to the activity under the optimum condition of the acid and alkaline region.

• Journal of the Korean Chemical Society
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• v.27 no.5
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• pp.353-360
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• 1983

The adsorption behavior of 8-hydroxyquinoline (8HQ) on Amberlite XAD-4 and-7 resins was investigated by measuring its distribution coefficients under various experimental conditions, such as shaking time, pH and concentration of methanol in the medium. The application of 8HQ-impregnated-XAD resins for the absorption and separation of metal ions was studied. The maximum adsorption of 8HQ on XAD resins was observed in the 30% methanol solution having pH range from 6.0 to 9.0. The impregnation capacities of XAD resins for 8HQ were 3.81${\times}$10-2mmol, 8HQ/g, XAD-4 resins and 2.60${\times}$10-2mmol, 8HQ/g, XAD-7 resin, respectively. The 8HQ-impregnated-XAD resins were stable in pH range from 6.0 to 10.0 and the amount of 8HQ leached from XAD-4 resin by eluting with hydrochloric acid(above 5M) was negligible. The optimum pH range for the adsorption of metal ions on 8HQ-impregnated XAD resin was also 6.0 to 10.0, and the adsorption mole ratio of metal ion to 8HQ were 1 : 2 for Cu(II), Cd(II) and Ni(II), and 1 : 3 for Fe(III) at the above pH range. It was found that the absorbed metal ions on 8HQ-impregnated-XAD resins were recovered quantitatively with 5M HCl and 8HQ-impregnated-XAD-4 resin could be reusable over 5 times without decrease in its impregnation capacity.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.9 no.3
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• pp.169-175
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• 1976

A solvent extraction-atomic absorption spectrophotometry for determination of trace amount of cadmium, copper, lead and zinc and a flameless atomic absorption spectrophotometry for mercury in sea water were studied. The optimum pH range for solvent extraction was pH 4-7. A better solvent extraction efficiency was obtained with MIBK solvent than nitrobenzene, benzene, isoamylalcohol, n-buthylacetate. DDTC was more advantageous than APDC as chelating agent. The metals, chelated with DDTC and concentrated into MIBK by solvent extraction with a volume of $1\iota$ of sea water for cadmium, copper and lead, and 200m1 for zinc, were determined simultaneously by atomic absorption spectrophotometry. For mercury determination, 500ml of sea water was digested with permanganate-sulfuric acid and mercury( II ) was reduced by stannous chloride and aerated the solution with air pump until the absorbance reached a constant value. The precisions, in standard deviation, of these methods were 0.058ppb for cadmium, 0.084 ppb for copper, 0.44ppb for lead, 2.49ppb for zinc and 0.08 ppb for mercury. The sensitivities, expressed in $ppb/1\%$ absorption, were 0.058 ppb cadmium, 0. 15 ppb copper, 0.6 ppb lead, 1.2 ppb zinc and 0.01 ppb mercury respectively. No significant adsorption on the wall of polyethylene sample bottle occurred during 30 days of storing by acidification to pH 1.5 with nitric acid except zinc. Poor reproducibility was found for zinc with this method.