• Korean Journal of Food Science and Technology
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• v.42 no.4
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• pp.390-397
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• 2010

Residual solvents in foods are defined as organic volatile chemicals used or produced in manufacturing of extracts or additives, or functional foods. The solvents are not completely eliminated by practical manufacturing techniques and they also may become contaminated by solvents from packing, transportation or storage in warehouses. Because residual solvents have no nutritional value but may be hazardous to human health, there is a need to remove them from the final products or reduce their amounts to below acceptable levels. The purpose of this study was to develop and evaluate an analytical method for the screening of residual solvents in health functional foods. Furthermore, the aim of this study was to constitute a reasonable management system based on the current state of the market and case studies of foreign countries. Eleven volatile solvents such as MeOH, EtOH, trichloroethylene and hexane were separated depending on their column properties, temp. and time using Gas Chromatography (GC). After determining the GC conditions, a sample preparation method using HSS (Head Space Sampling) was developed. From the results, a method for analyzing residual solvents in health functional foods was developed considering matrix effect and interference from the sample obtained from the solution of solvents-free health functional foods spiked with 11 standards solutions. Validation test using the developed GC/HSS/MS (Mass Spectrometry) method was followed by tests for precision, accuracy, recovery, linearity and adequate sensitivity. Finally, examination of 104 samples grouped in suits was performed by the developed HSS/GC/MS for screening the solvents. The 11 solvents were isolated from health functional foods based on vapor pressure difference, and followed by separation within 15 minutes in a single run. The limt of detection (LOD), limit of quantification (LOQ), recovery and coefficient of variation (C.V.) of these compounds determined by the HSS/GC/MS were found to be 0.1 pg/mL, 0.1-125 pg/g, 51.0-104.6%, and less than 15%, respectively. Using the developed HSS/GC/MS method, residual solvent from 16 out of 104 health functional products were detected as a EtOH. This method therefore seems t o be a valuable extension ofanalytical method for the identification of residual solvents in health functional food.

• Food Science of Animal Resources
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• v.32 no.5
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• pp.571-577
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• 2012

This study was carried out to develop an analytical method for the determination of vitamin D in infant formula. Vitamin D was determined by column-switching high-performance liquid chromatography (HPLC) equipped with a reversed phase column and UV detector after saponification and extraction of the formula with an organic solvent. A preseparation column ($C_8$), focusing column ($C_{18}$), analytical column ($C_{18}$) and UV-Vis detector (254 nm) were used. The limits of detection (LOD) and the limits of quantification (LOQ) for vitamin D were estimated to be $1.51{\mu}g/kg$ and $4.95{\mu}g/kg$, respectively. The linearity, recovery, precision and accuracy of the analytical method for vitamin D were evaluated through the application of a SRM (Standard Reference Material) 1846 (National Institute of Standard & Technology, USA). The linearity of this method was calculated with a value of the coefficient of determination ($r^2$) ${\geq}0.9999$. The recovery of vitamin D was $85.20{\pm}3.00%$. The intra-assay precision for vitamin D was between $1.68{\pm}0.03%$ and $5.75{\pm}0.33%$, and the inter-assay precision for vitamin D ranged from $1.73{\pm}0.03%$ to $2.96{\pm}0.09%$. The intra-assay accuracy for vitamin D was between $100.03{\pm}2.77%$ and $102.01{\pm}0.59%$, and the inter-assay accuracy for vitamin D ranged from $99.00{\pm}1.53%$ to $102.01{\pm}3.04%$. The proposed method is optimal for the separation and quantification of vitamin D from infant formula.

• Korean Journal of Environmental Agriculture
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• v.21 no.2
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• pp.90-95
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• 2002

A study was carried out to optimize the cleanup step using a solid-phase extraction (SPE) cartridge, $SupelClean^{TM}$ Florisil, for multiresidue analysis of 16 pesticides in cucumber matrix. Eluting efficiencies of two solvent systems including acetone/n-hexane and ethyl acetate/n-hexane mixtures were critically evaluated by recoveries of target anaytes from the SPE Florisil column. Based on the recovery as a measure of eluting efficiency, an acetone/n-hexane (20/80,v/v) mixture provided more than 80% recovery for 15 pesticides except bifenthrin. In case of ethyl acetate/n-hexane, 14 pesticides showed recoveries higher than 75% while those far alachlor and bifenthrin were less than 30%.

• Korean Journal of Food Science and Technology
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• v.4 no.4
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• pp.252-258
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• 1972

Methods of separating yeast cells from oil-water-cell emulsion and subsequent purification of the recovered yeast have been studied. In addition, the results of preliminary feeding experiments in which a yeast grown on gas oil was incorporated into chick rations are reported. According to the present study, it appears that the recovery of the yeasts would be easier at pH 9, since the emulsion is relatively more unstable. A class of surface active agent at a concentration of 0.3% was found to facilitate the separation of the yeast from the emulsion. The use of electrolytes such as NaCl and KCl were found to be most effective in breaking the emulsion. Solvent treatment using iso-propyl alcohol and its azeotropic mixture with hexane at $58^{\circ}C$ are particularly suitable for purification of the yeast. In the feeding experiment it was found that 5 percent of the fishmeal in the control ration could be replaced by the yeast with no adverse effect on performance. However, when 8 percent of the fish meal in the control ration was replaced by the yeast, some effect on live-weight gain of the chicks was observed.

• Membrane Journal
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• v.26 no.3
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• pp.220-228
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• 2016

Carbon molecular sieve (CMS) hollow fiber membranes were prepared by carbonizing a polyimide precursor manufactured by non-solvent induced phase separation process. Gas separation performance of CMS hollow fiber membrane was investigated on the effect of three carbonization conditions. CMS membrane with the highest gas separation performance was obtained at the pyrolysis temperature of $250-450^{\circ}C$: $N_2$, $SF_6$, and $CF_4$ permeance were 20, 0.32, 0.48 GPU, respectively, and $N_2/SF_6$ and $N_2/CF_4$ selectivities were 62 and 42, respectively. In the $SF_6/CF_4/N_2$ mixture gas test, when the stage cut was 0.2, the recovery ratio of $SF_6$ and $CF_4$ was over 99% and 98%. $SF_6$ concentration ratio was 4.5 times higher than the $SF_6$ concentration at the feed side. From the results, it was concluded that CMS membrane was one of the promising membranes for recovery Perfluorocompound gases process.

• Journal of Food Hygiene and Safety
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• v.29 no.4
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• pp.312-315
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• 2014

The present study demonstrated the development and validation of the method for the quantification of phenol in food using gas chromatography coupled with mass spectrometry (GC-MS). After spiking of internal standard (Phenol-$d_5$) to food, those samples were extracted with organic solvent mixture (acetone : dichloromethane = 1 : 1, v/v) using ultra sonic extractor and cleaned by gel permeation chromatography (GPC) technique. The amount of phenol was determined by GC/MS. To validate the developed method, we evaluated parameters were the selectivity, linearity, accuracy, precision, and recovery. To demonstrate the selectivity of the method, blank samples of rice, corn, and fish(mackerel) were prepared and subjected to GC-MS analysis. To verify the linearity of the method, six different standard concentrations of phenol at 0.01, 0.05, 0.1, 0.5, 1 and 2.5 mg/kg were evaluated. The correlation coefficient ($r^2$) of calibration curve was 0.9999. The recovery rate for phenol standard calculated by internal standard method were 82.2~101.5% for samples fortified with 0.25, 0.50, and 1.0 mg/kg, respectively. Also the repeatability and reproducibility for validation of precision were 0.2~5.5%. According to the result of the validation, this established method was suitable for AOAC guideline. The limit of detection (LOD) for phenol analysis were 0.03~0.1 mg/kg, and the limit of quantification (LOQ) were 0.1~0.3 mg/kg. Therefore, we established the optimal analysis method for determination of phenol in food using GPC and GC/MS.

• Korean Chemical Engineering Research
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• v.43 no.5
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• pp.641-645
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• 2005

Using aqueous solution of 60% ethanol, the isoflavones contained in the Soybean (Chungsun, Korea), Tawon (Suwon, Korea), Jackbean (Hongsung, Korea), Soybean (Jilin, China), Black Soybean (Jilin, China), Kidneybean (Jilin, China) and Soybean (California, U.S.A.) were extracted. In this work, the pretreatment step was composed of agitation extraction, filtration, concentration, ultracentrifuge, and membrane filtration. The analysis by $C_{18}$ column was performed, and the mobile phase applied was linearly changed with A/B of 85/15-65/35 vol% for 50 min (A water/acetic acid, 99.9/0.1 vol%, B acetonitrile/acetic acid, 99.9/0.1 vol%). Among the soybeans tested, the total amounts of the four isoflavones (daidzin, genistin, daidzein, and genistein) extracted by the soybeans from Korea, China and U.S.A. were 1.37, 1.60, and 2.25 mg/g, respectively. It was also found that the total amount of aglycone of daidzein and genistein from soybean (American California) was $144{\mu}g/g$, which was the largest for the soybeans experimented.

• Resources Recycling
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• v.30 no.6
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• pp.28-35
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• 2021

An experiment was conducted to separate or recover Co and Ni using Cyanex 301 from process by-products and waste resources containing Co and Ni. To separate and recover Co and Ni from simulated leaching solutions, 10 v/v% Cyanex 301 was used as an extractant in this study; Li was not extracted. At equilibrium pH 1.5 and a phase ratio (A/O) of 1.0, 0.44% of Mg and 11.57% of Mn were extracted, and more than 99% of Co and Ni were extracted. McCabe-Thiele diagram analysis confirmed that more than 99.9% of Co and Ni could be extracted simultaneously through two-stage extraction with an extraction phase ratio (A/O) of 2. It was possible to extract Mg and Mn simultaneously through the scrubbing process. In the scrubbing process, more than 99% of Mg and 87% of Mn were scrubbed using 0.05 M of H₂SO₄, and 99.9% of Mg and more than 80% of Mn were scrubbed using 0.05 M of HCl. In the stripping process, 93% of Co and 5% of Ni were stripped selectively by 3.0 M of H₂SO₄. However, when 8.0 M of HCl was used as a stripping solution, more than 99.9% of Co and more than 90% of Ni were stripped simultaneously.

• Clean Technology
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• v.25 no.1
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• pp.14-18
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• 2019

In general after the etching process, waste etching solution contains metals. (ex. Nickel (Ni), Chromium (Cr), Zinc (Zn), etc.) In this work, we proposed a recycling process for waste etching solution and refining from waste liquid contained nickel to make nickel metal nano powder. At first, the neutralization agent was experimentally selected through the hydrolysis of impurities such as iron by adjusting the pH. We selected sodium hydroxide solution as a neutralizing agent, and removed impurities such as iron by pH = 4. And then, metal ions (ex. Manganese (Mn) and Zinc (Zn), etc.) remain as impurities were refined by D2EHPA (Di-(2-ethylhexyl) phosphoric acid). The nickel powders were synthesized by liquid phase reduction method with hydrazine ($N_2H_4$) and sodium hydroxide (NaOH). The resulting nickel chloride solution and nickel metal powder has high purity ( > 99%). The purity of nickel chloride solution and nickel nano powders were measured by EDTA (ethylenediaminetetraacetic) titration method with ICP-OES (inductively coupled plasma optical emission spectrometer). FE-SEM (field emission scanning electron microscopy) was used to investigate the morphology, particle size and crystal structure of the nickel metal nano powder. The structural properties of the nickel nano powder were characterized by XRD (X-ray diffraction) and TEM (transmission electron microscopy).

• Journal of the Korean Chemical Society
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• v.30 no.5
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• pp.423-432
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• 1986

Atomic absorption spectrophotometric (AAS) determination of hexavalent chromium [Cr(VI)] in a waste water was studied. Cr(VI) was extracted with p-xylene from the wastewater, in the way of ion pair formation with anion exchanger aliquat-336(tri-caprylmethyl ammonium chloride). 100ml waste water, after organic materials were extracted out with toluene, was acidified with conc. HCl adjusting the medium to pH 0.5 and 20ml of p-xylene containing 0.01M aliguat-336 was used to extract Cr(VI) from the acidified solution. The absorbance of chromium was measured with air-acetylene flame at 357.9nm. Standard addition method was used in the determining concentration of Cr(VI) extracted. No interference has been found in the extraction of Cr(VI) by the Al(III), Fe(III) and Cr(III) ion presented. However, Fe(II) decreased the absorbance of Cr(VI), due to the fact Fe(II) reduces Cr(VI) to Cr(III). The contained organic material was removed prior to extracting process, since it may reduced the absorbance of Cr(VI). The recovery of added Cr(VI) was over 96%, which seems to be promising and the relative standard deviation was 3.95%