• Title/Summary/Keyword: Acid extraction

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Development of Simultaneous Analytical Method of Veterinary Antibiotics in Manure using Liquid Chromatography Coupled with Tandem Mass Spectrometry (LC-MS/MS를 이용한 퇴비 및 액비 중 항생제 동시 분석법 개발)

  • Chung, Hyung Suk;Lee, Young Jun;Lee, Han Sol;Rahman, Md. Musfiqur;Kabir, Md. Humayun;Park, Byung-Jun;Kim, Jang-Eok;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.36 no.3
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    • pp.201-210
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    • 2017
  • BACKGROUND: The current study was to monitor of 9 veterinary antibiotics (ceftiofur, clopidol, florfenicol, sulfamethazine, sulfamethoxazole, sulfathiazole, tetracycline, tiamulin, and tylosin) in manure using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive and negative electrospray ionization mode. METHODS AND RESULTS: Sample preparation was carried out using Mcllvaine buffer and citrate salts to adjust the pH of the sample followed by purification with dispersive solid phase extraction (d-SPE). Separation of analytes during LC-MS/MS analysis was conducted using an Eclipse Plus $C_{18}$ column and the mobile phase was in gradient mode with, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations of all tested antibiotics was good, with $R^2$ determination coefficients ${\geq}0.9920$. The limit of detection (LOD) and quantifications (LOQ) were $0.1-67.0{\mu}g/kg$ and $0.4-200.0{\mu}g/kg$, respectively. Analysis of 13 solid and liquid manure samples taken from the Republic of Korea revealed concentrations less than $0.7{\mu}g/kg$ for tiamulin, $1497.6{\mu}g/kg$ for sulfamethazine. CONCLUSION: To monitor 9 veterinary antibiotics from manure samples in 13 provincial areas throughout the Republic of Korea, an analytical method was developed. The developed method was fully validated and successfully applied for monitoring various veterinary antibiotics in manure samples.

Inhibitory Effect of Cell Differentiation against 3T3-L1 Pre-Adipocytes and Angiotensin Converting Enzyme (ACE) Activity of Ice Plant (Mesembryanthemum crystallinum) (아이스플랜트(Mesembryanthemum crystallinum)의 3T3-L1 전지방세포 분화 및 Angiotensin-Converting Enzyme(ACE) 활성 억제)

  • Kang, Seung Mi;Kim, Seon Jeong;Nam, Sanghae
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.8
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    • pp.1012-1017
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    • 2017
  • Mesembryanthemum crystallinum (Family: Aizoaceae) is an annual plant consisting of ice crystal-shaped bladder cells, which is responsible for its common name ice plant. This study investigated biological activities according to general components and extraction solvent in order to examine the functionality of ice plant. The total content of free amino acids was 32.57 mg/g, including 4.64 mg/g of L-alanine as the most abundant and 2.60 mg/g of ${\gamma}$-aminobutyric acid. Regarding angiotensin converting enzyme inhibitory activities of solvent fractions of ice plant, ethyl acetate fraction and chloroform fraction showed activities of $33.17{\pm}3.20{\sim}88.19{\pm}3.20%$ and $23.72{\pm}2.89{\sim}86.78{\pm}2.24%$, respectively, similar to $Captopril^{(R)}$ ($19.51{\pm}3.44{\sim}84.72{\pm}1.06%$) and $Enalapril^{(R)}$ ($24.93{\pm}1.12{\sim}91.32{\pm}3.62%$) as positive control groups. Regarding inhibition of lipid droplet production in 3T3-L1 preadipocytes by ice plant, anti-adipogenic activities were $53.00{\pm}0.45{\sim}65.75{\pm}0.31%$ and $44.16{\pm}0.29{\sim}63.32{\pm}0.36%$ in the ethyl acetate fraction and butanol fraction, respectively, showing the lowest lipid droplet production. The chloroform fraction and hexane fraction showed activities of $38.33{\pm}0.09{\sim}56.55{\pm}0.50%$ and $31.17{\pm}0.50{\sim}55.10{\pm}1.93%$, respectively, whereas the water fraction showed activity of $26.32{\pm}2.27{\sim}49.48{\pm}0.05%$. Therefore, all solvent fractions inhibited fat accumulation of 3T3-L1 preadipocytes according to treatment concentration. According to the results above, it would be possible to utilize ice plant as a new health functional material.

Establishment of Biotin Analysis by LC-MS/MS Method in Infant Milk Formulas (LC-MS/MS를 이용한 조제유류 중 비오틴 함량 분석법 연구)

  • Shin, Yong Woon;Lee, Hwa Jung;Ham, Hyeon Suk;Shin, Sung Cheol;Kang, Yoon Jung;Hwang, Kyung Mi;Kwon, Yong Kwan;Seo, Il Won;Oh, Jae Myoung;Koo, Yong Eui
    • Journal of Food Hygiene and Safety
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    • v.31 no.5
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    • pp.327-334
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    • 2016
  • This study was conducted to establish the standard method for the contents of biotin in milk formulas. To optimize the method, we compared several conditions for liquid extraction, purification and instrumental measurement using spiked samples and certified reference material (NIST SRM 1849a) as test materials. LC-MS/MS method for biotin was established using $C_{18}$ column and binary gradient 0.1% formic acid/acetonitrile, 0.1% formic acid/water mobile phase is applied for biotin. Product-ion traces at m/z 245.1 ${\rightarrow}$ 227.1, 166.1 are used for quantitative analysis of biotin. The linearity was over $R^2=0.999$ in range of $5{\sim}60{\mu}g/L$. For purification, chloroform was used as a solvent for eliminating lipids in milk formula. The linearity was over 0.999 in range of 5~60 ng/mL. The detection limit and quantification limit were 0.10, 0.31 ng/mL. The accuracy and precision of LC-MS/MS method using CRM were 103%, 2.5% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested milk formulas were acceptable contents of biotin compared with component specification and standards for nutrition labeling. The standard operating procedures were prepared for biotin to provide experimental information and to strengthen the management of nutrient in milk formula.

Investigating The Potential of Human Hair Produced from The Beauty Parlor and Barbershop as a Raw Material of Wood Adhesives (미·이용업 폐기물 인모의 목재접착제 원료화 가능성 탐색)

  • Yang, In;Ahn, Sye Hee
    • Journal of the Korean Wood Science and Technology
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    • v.45 no.5
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    • pp.599-612
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    • 2017
  • Human hair (HH) is produced as a waste from beauty parlor and barbershop. HH-based adhesives were formulated with NaOH-hydrolyzed HH, $H_2SO_4$-hydrolyzed chicken blood (CB) and PF as a crosslinking agent. Physicochemical properties and retention rate against hot water of the adhesives were measured to investigate the potential of HH as a raw material of wood adhesives. HH was composed of keratin-type protein of 80% and over. Ash of less than 0.1% was contained in HH. Among the amino acids included in HH, glutamic acid showed the highest content, followed by cysteine, serine, arginine and threonine. Solid content of the adhesives ranged from 33.2% to 41.8% depending on hydrolysis conditions of HH and PF type. Viscosity at $25^{\circ}C$ ranged from 300 to $600mPa{\cdot}s$ resulting in a sprayable adhesive. Retention rate against hot water measured to evaluate the water resistance of adhesives was the highest in the cured resin formulated with 5% NaOH-hydrolyzed HH and 5% $H_2SO_4$-hydrolyzed CB. Meanwhile, the molar ratio of formaldehyde to phenol in PF did not have a significant impact on the retention rate of HH-based adhesives. When the retention rates of HH-based adhesives were compared to those of conventional wood adhesive resins used for the production of wood-based panels extensively, HH-based adhesives formulated with 30 wt% PF showed lower retention rate than commercial urea-formaldehyde resin. However, when PF content was increased to 35 wt%, the retention rate greatly increased and approached to that of commercial melamine-urea-formaldehyde resin. Except for the results mentioned above, the analysis of economic feasibility suggests that HH-based adhesives can be used for the production of wood-based panels if HH is hydrolyzed in proper conditions and then the HH-based adhesives are formulated by the HH hydrolyzates with 35 wt% PF.

Comparison of Anti-Oxidative Activities of Gamma-Irradiated Aralia continentalis Extracts for Long-Term Storage of Oriental Medicine (한약재 장기 보존을 위해 감마선 조사한 독활(Aralia continentalis) 추출물의 항산화 효과 비교)

  • Park, Hye-Jin;Hong, Eun-Jin;Hong, Shin-Hyub;Cho, Young-Je
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.1
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    • pp.46-55
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    • 2017
  • In this study, extracts of gamma-irradiated Aralia continentalis for health and beauty food resources were examined on antioxidant activities and increasing extraction yield. In photostimulated luminescence analysis, non-irradiated (0 kGy) sample showed an intermediate result of 891.00 photon counts (PCs), whereas irradiated (5 and 10 kGy) samples showed positive results of 79,956.67 and 282,498.67 PCs, respectively. The thermoluminescence ratio of non-irradiated samples was 0.018, whereas the values of irradiated samples (5 and 10 kGy) were 0.395 and 0.464, respectively. Electron spin resonance (ESR) analysis as a physical technique for irradiation identification of Aralia continentalis showed a pair of peaks on a space of 6.0 mT in the symmetric ESR spectrums. For phenolics of gamma-irradiated Aralia continentalis, water extracts had the highest amounts of 7.61 mg/g at non-irradiated condition (0 kGy) while 50% ethanol extracts had the highest amounts of 6.86 mg/g at 10 kGy irradiation. 2,2-Diphenyl-1-picrylhydrazyl scavenging activity of water and 50% ethanol extracts from non-irradiated and irradiated Aralia continentalis were very high (94.99~100.00%). 2,2'-Azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) radical cation inhibitory activity was over 95.00% at $200{\mu}g/mL$ phenolics. Antioxidant protection factor (PF) showed a very high level of activity (1.38~2.51 PF). Thiobarbituric acid reactive substance inhibitory activity was high (70% and 95%, respectively). Thus, treatment of gamma irradiation can be used as a method of storage for long-term preservation of Oriental medicine.

Purification and Characterization of Oriental Pear(Niitaka, Pyrus pyrifolia Nak.) Protease (동양배(신고(新高)) Protease의 정제(精製) 및 성질(性質)에 관(關)하여)

  • Kim, Seung Yeol;Chung, Hai Jung;Kim, Seung Kyeom;Shin, Cheol Seung
    • Korean Journal of Agricultural Science
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    • v.16 no.2
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    • pp.225-238
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    • 1989
  • These studies were conducted to investigate the extraction, purification and characterization of oriental pear (Niitaka. Pyrus pyrifolia Nak.) protease, and the results obtained were as follows: 1. Oriental pear protease was effectively extracted by the method of homogenizing pear pulp with 0.7 volume of 0.1M-sodium phosphate buffer, pH 6.5 containing 5mM-cysteine, 40mM-2-mercaptoethanol and 2mM-EDTA at 10,000 rpm for 5 min. 2. The protease was purified by ammonium sulfate fractionation, Sephadex G-100 filtration and DEAE-Sephadex A-50 column chromatography, and the purified enzyme gave a single protein band on polyacrylamide gel electrophoresis. 3. The specific activity of purified enzyme was 29.65 unit/mg protein and the yield was 7.22%. 4. The moecular weight of the protease was estimated to be about 51,000 by SDS-polyacrylamide gel electrophoresis, and the enzyme had Km value of 54.5 mg/ml for casein. 5. The purified enzyme had a maximum activity at pH 6.0 and $50^{\circ}C$, and was stable from pH 5.5-6.5 and at temperatures below $50^{\circ}C$ 6. Casein was a better substrate for this protease compared to hemoglobin. 7. The enzyme activity was markedly inhibited by p-chloromercuribenzoic acid and heavy metal salts such as $HgCl_2$ and $MnSO_4$ also considerably inhibited the enzyme activity.

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Anti-aging Effect of Inula britannica var. chinensis Flower Extract According to the Extraction Temperature (추출 온도에 따른 금불초 꽃 추출물의 항노화 효능)

  • Jeon, Ji Min;Yoo, Dae Sung;Cheon, Jong Woo;Kwon, Soon Sik;Jeon, So Ha;Park, Soo Nam
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.40 no.1
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    • pp.109-120
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    • 2014
  • In this study, the extracts of Inula britannica var. chinensis (I. britannica) flower were extracted at three different temperatures (room temperature, $45^{\circ}C$, and $65^{\circ}C$) and their anti-aging effects were studied. Before investigating anti-aging effects of the extracts, their cytotoxicity was tested on B16F10, Hs683, and HaCaT cells. All extracts showed no cytotoxicity at the concentration less than 0.1% (v/v). Melanin synthesis inhibitory activities in B16F10 cells and reverse transcriptase polymerase chain reaction (RT-PCR) in Hs683 and HaCaT cells were used to see their anti-aging effects. The room temperature extract at 0.1% showed 24.5% melanin synthesis inhibition, which was better than the $45^{\circ}C$ and $65^{\circ}C$ extracts. In addition, expression rates of the room temperature extract at 0.1% on HAS-1, HAS-2, and HAS-3 related to hyaluronan synthase genes were 123.3%, 137.8%, 133.2%, respectively. which were higher than reference material of L-ascorbic acid. Expression rates of the $45^{\circ}C$ extract at 0.1% on TNF-${\alpha}$, COX-2, and IL-$1{\alpha}$, which are inflammatory related genes, was suppressed to 30.3%, 12.8%, 25.7%, respectively. It was better in anti-in flammatory effect than the room temperature and $65^{\circ}C$ extracts. As results, we showed that I. britannica var. chinensis flower extarcts decreased melanin production and expression of inflammatory related genes and increased the expression rate of hyaluronan synthase genes. Thus, it is believed that the extracts affect anti-aging effects of skin through whitening, moisturizing, and anti-inflammatory processes and could be applicable to cosmetics as a functional cosmetic ingredient.

Characterization of Arsenic Immobilization in the Myungbong Mine Tailing (명봉광산의 광미 내 비소의 고정화 특성 연구)

  • Lee, Woo-Chun;Jeong, Jong-Ok;Kim, Ju-Yong;Kim, Soon-Oh
    • Economic and Environmental Geology
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    • v.43 no.2
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    • pp.137-148
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    • 2010
  • The Myoungbong mine located in Boseong-gun, Jellanamdo consists of Au-Ag bearing quartz veins which filled the fissures of Bulguksa granitic rocks of Cretaceous. The tailings obtained from the Myungbong mine were used to investigate the effects of various processes, such as oxidation of primary sulfides and formation(alteration) of secondary and/or tertiary minerals, on arsenic immobilization in tailings. This study was conducted via both mineralogical and chemical methods. Mineralogical methods used included gravity and magnetic separation, ultrasonic cleaning, and instrumental analyses(X-ray diffractometry, energy-dispersive spectroscopy, and electron probe microanalyzer) and aqua regia extraction technique for soils was applied to determine the elemental concentrations in the tailings. Iron (oxy)hydroxides formed as a result of oxidation of tailings were identified as three specific forms. The first form filled in rims and fissures of primary pyrites. The second one precipitated and coated the surfaces of gangue minerals and the final form was altered into yukonites. Initially, large amounts of acid-generating minerals, such as pyrite and arsenopyrite, might make the rapid progress of oxidation reactions, and lots of secondary minerals including iron (oxy)hydroxides and scorodite were formed. The rate of pH decrease in tailings diminished, in addition, as the exposure time of tailings to oxidation environments was prolonged and the acid-generating minerals were depleted. Rather, it is speculated that the pH of tailings increased, as the contribution of pH neutralization reactions by calcite contained in surrounding parental rocks became larger. The stability of secondary minerals, such as scorodite, were deteriorated due to the increase in pH, and finally arsenic might be leached out. Subsequently, calcimn and arsenic ions dissociated from calcites and scorodites were locally concentrated, and yukonite could be grown tertiarily. It is confirmed that this tertiary yukonite which is one of arsenate minerals and contains arsenic in high level plays a crucial role in immobilizing arsenic in tailings. In addition to immobilization of arsenic in yukonites, the results indicate that a huge amount of iron (oxy)hydroxides formed by weathering of pyrite which is one of typical primary minerals in tailings can strongly control arsenic behavior as well. Consequently, this study elucidates that through a sequence of various processes, arsenic which was leached out as a result of weathering of primary minerals, such as arsenopyrite, and/or redissolved from secondary minerals, such as scorodite, might be immobilized by various sorption reactions including adsorption, coprecipiation, and absorption.

Etiological Properties and Coat Protein Gen Analysis of Potato Virus Y Occuring in Potatoes of Korea (우리나라 감자에 발생하는 PVY의 병원학적 특성 및 외피단백질 유전자 분석)

  • ;Richard M. Bostock
    • Proceedings of the Korean Society of Plant Pathology Conference
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    • 1995.06b
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    • pp.77-96
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    • 1995
  • To obtain basic informations for the improvement of seed potato production in Korea, some etiological properties of potato virus Y(PVY) distributed in the major seed potato production area(Daekwanryeong) were characterized, and the nucleotide and amino acid sequences of the coat protein gene of the PVY strains isolated were analyzed. PVY strains in Daekwonryeong, an alpine area, were identified to be two strains, PVYo and PVYN by symptoms of indicator plants, and their distribution in potato fields was similar. Major symptom on potato varieties by PVY was grouped as either mosaic alone or mosaic accompanied with veinal necrosis in the lower leaves. The symptom occurrence of the two symptoms was similar with Irish Cobbler, but Superior showed a higher rate of mosaic symptom than the other. The PVY strain which was isolated from potato cv. Superior showing typical mosaic symptoms produced symptoms of PVY-O on the indicator plants of Chenopodium amaranticolor, Nicotiana tabacum cv. Xanthi nc and Physalis floridana, but no symptom o Capsicum annum cv. Ace. Moreover, results from the enzyme-linked immunosorbent assay with monoclonal and polyclonal antibodies showed that the isolated PVY reacts strongly with PYV-O antibodies but does not react specifically with PVY-T antibodies. The purified virus particles were flexious with a size of 730$\times$11nm. On the basis of the above characteristics, the strain was identified to be a PVY-O and named as of PVY-K strain. The flight of vector aphids was observed in late May, however, the first occurrence of infected plants was in mid June with the bait plants surrounded with PVY-infected potato plants and early July with the bait plants surrounded with PVY-free potato plants. PVY infection rates by counting symptoms on bait plants (White Burley) were 1.1% with the field surrounded with PVY-free potato plants and 13.7% the fields surrounded with PVY-infected potato plants, showing the effect of infection pressure. The propagated PVY-K strain on tobacco(N. sylvestris) was purified, and the RNA of the virus was extracted by the method of phenol extraction. The size of PVY-K RNA was measured to be 9, 500 nucleotides on agarose gel electrophoresis. The double-stranded cDNAs of PVY-K coat protein(CP) gene derived by the method of polymerase chain reaction were transformed into the competent cells of E. coli JM 109, and 2 clones(pYK6 and pYK17) among 11 clones were confirmed to contain the full-length cDNA. Purified plasmids from pYK17 were cut with Sph I and Xba I were deleted with exonuclease III and were used for sequencing analysis. The PVY-K CP gene was comprised of 801 nucleotides when counted from the clevage site of CAG(Gln)-GCA(Ala) to the stop codon of TGA and encoded 267 amino acids. The molecular weight of the encoded polypeptides was calculated to be 34, 630 daltons. The base composition of the CP gene was 33.3% of adenine, 25.2% of guanine, 20.1% of cytosine and 21.4% of uracil. The polypeptide encoded by PVY-K CP gene was comprised of 22 alanines, 20 threonines, 19 glutamic acids and 18 glycines in order. The homology of nucleotide sequence of PVY-K CP gene with those of PVY-O(Japan), PVY-T(Japan), PVY-TH(Japan), PVYN(the Netherlands), and PVYN(France) was represented as 97.3%, 88.9%, 89.3%, 89.6% and 98.5%, respectively. The amino acid sequence homology of the polypeptide encoded by PVY-K CP gene with those encoded by viruses was represented as 97.4%, 92.5%, 92.9%, 92.9%, and 98.5%, respectively.

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Characteristics of Pop-rice and Rice Tea Using Black Sticky Rice with Giant Embryo (흑찰거대배아미를 이용한 팝라이스와 흑미차의 품질 특성)

  • Han, Sang-Ik;Seo, Woo Duck;Na, Ji-Eun;Park, Ji-Young;Park, Dong-Soo;Cho, Jun-Hyun;Lee, Jong-Hee;Seo, Kyung-Hye;Sim, Eun-Yeong;Nam, Min-Hee
    • Journal of Life Science
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    • v.25 no.1
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    • pp.68-74
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    • 2015
  • Recently developed black waxy rice with a giant embryo ('Nunkeunheukchal', BGE) was selected and processed to produce high quality nutritional food. BGE contains high levels of several phytochemicals with antioxidant activities, as well as other reported health beneficial properties. In addition, the giant embryo has high protein, lipid, and amino acids contents. Within the free amino acids, ${\gamma}$-aminobutyric acid (GABA), a major inhibitory neurotransmitter, has long been used for treating the aftereffects of brain injuries and stroke. A method for manufacturing pop-rice and black rice tea by popping process in BGE is provided to increase a taste, nutrition and functionality. The produced 'pop-rice' showed increased protein (11.3%) and lipid (3.7%) contents compared with control variety, IB ('Ilmibyeo'). In addition, melanoidin related products, polyphenol and functional amino acid contents were increased by the popping process. Pop-rice tea made of BGE showed the highest extraction of total sugar, glucose, raffinose and sucrose (4 times higher than brown rice) by hot water. Scavenging activity ($SC_{50}$) of processed BGE rice powder showed strong antioxidative activity of 0.24 mg/ml using DPPH and 1.82 mg/ml using ABTs method. Thereafter, these results suggested that the popping processed rice of BGE could be one of the promising materials for healthy food development.