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Simultaneous Analysis for Veterinary Drug Residues in Honey by HPLC/MS/MS (HPLC-MS/MS를 이용한 벌꿀 중 동물용의약품 동시분석방법 연구)

  • Kim, Jong-Hwa;Moon, Sun-Ea;Kim, Ki-Yu;Jung, You-Jung;Lee, Chang-Hee;Ku, Eun-Jung;Yoon, Mi-Hye;Lee, Jong-Bok
    • Journal of Food Hygiene and Safety
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    • v.31 no.2
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    • pp.94-98
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    • 2016
  • This study was conducted to establish the simultaneous analysis method for veterinary drug residues in honey by high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS). The eleven targeting veterinary drugs with honey test method in Korean Food Standards Codex were divided into Group 1 (streptomycine dihydrostreptomycine, neomycine) and Group 2 (oxytetracycline, enrofloxacin, ciprofloxacin, cymiazole, chloramphenicol, amitraz, coumaphos, fluvalinate) to be analyzed simultaneously. From the results, the retention time (RT) of the targeting drugs was within 15 min, the range of detection limits was 0.0056 to $0.0643{\mu}g/g$ and the range of quantification limits was 0.0169 to $0.1948{\mu}g/g$. The coefficients of determination ($R^2$) for Group 1 ($0.05{\sim}1.0{\mu}g/mL$) and Group 2 ($0.01{\sim}1.0{\mu}g/mL$) were 0.9917~0.9987 and 0.9923~1.000 respectively, and showed the good linearity. The recovery rates for Group 1 (final conc. $0.25{\mu}g/g$) and Group 2 (final conc. $1.0{\mu}g/g$) were 65.1~80.6% and 64.2~90.3% respectively. Also, the analysis results of inter day (n = 3) and intra day (n = 6) RSD (%) for area and retention time showed that the RSD (%) for area and retention time was below 10.92% and 1.57%. Therefore, the simultaneous analysis method of this study is evaluated to be a good test method for veterinary drug residues in honey.

Isolation and Chemical Analysis of Potent Anti-Complementary Polysaccharides from Fruiting Bodies of the Fomes fomentarius (말굽버섯 자실체에서 분리한 항보체 활성 다당체의 화학적 분석)

  • Park, Jung-Keun;Park, Kwe-Won;Shin, Kwang-Soon;Lee, Chang-Muk;Seok, Soon-Ja;Kim, Jeong-Bong;Koo, Bon-Sung;Han, Bum-Soo;Yoon, Sang-Hong
    • Microbiology and Biotechnology Letters
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    • v.41 no.2
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    • pp.198-206
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    • 2013
  • The five anti-complementary polysaccharides (MFKF-NP, MFKF-AP1${\alpha}$, ${\beta}$, and MFKF-AP2${\alpha}$, ${\beta}$) were separated from hot water extracts of fruiting bodies of Fomes fomentarius by two subsequent column chromatography using DEAE-sepharose FF and Concanavalin A-sepharose 4B. The order of anti-complementary activity was MFKF-AP1${\beta}$ > MFKF-AP1${\alpha}$ > MFKF-AP2${\alpha}$ > MFKF-AP2${\beta}$ > MFKF-NP > Polysaccharide Krestine (PSK). Especially, MFKF-AP1${\beta}$ among those showed the most excellent anti-complementary activity (70% of ITCH50 value at $20{\mu}g/ml$). The monosaccharide composition analysis by gas chromatography indicates that MFKF-AP1${\alpha}$ and ${\beta}$ are a kind of homoxylan consisted mainly of xylose above 97%. Molecular weight of MFKF-AP1${\beta}$, major anti-complementary polysaccharide, was estimated to be about 12,000 by high performance liquid chromatography (HPLC). After the incubation of the serum with MFKF-AP1${\beta}$ in the presence or absence of $Mg^{++}$ and $Ca^{++}$ ions, its anti-complementary activity was investigated. This result indicated that MFKF-AP1${\beta}$ seems to be activator both on the classical and the alternative pathway of complement activation.

Studies on the Composition of Fatty Acid in the Lipid Classes of Seed Oils of the Labiatae Family (순형과(脣形科) 종실유(種實油)의 지질분획별(脂質分劃別) 지방산(脂肪酸) 조성(組成)에 관한 연구(硏究))

  • Joh, Yong-Goe;Lee, Ok-Kyoung;Lim, Young-Ju
    • Journal of the Korean Applied Science and Technology
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    • v.5 no.1
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    • pp.13-23
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    • 1988
  • Contents of total lipids, neutral lipids, glycolipids and phospholipids of seed oils of 16 species of the Labiatae family were determined and their fatty acid compositions were analyzed by gas-liquid chromatography. The results were summarized as follows. 1) Lipid contents of seeds were shown to be 40.6% in Perilla frutescens Britton var. japonica, 32.2% in P. frutescens britton var. acuta, 31.9% in lsodon japonicus, 32.7% in l. inflexus, 48.3% in l. serra, 35.1% in Mosls dianthera, 38.2% in M. punctulata, 33.4% in Nepeta cataria, 26.3% in Agastache rugosa, 30.9% in Eisholtzia ciliata, 18.9% in Salvia splendens, 23.9% in Lycopus maackianus, 49.5% in Clinopodium chinense var. parviflorum, 30.9% in Ametystea caerulea, 33.1% in Leonurus sibircus and 34.3% in Scutellaria basicalensis. 2) Contents of neutral lipids, glycolipids and phospholipids from the seed oils amounted to 98.6%, 0.7%, 0.8% in P. frutescens Britton var. japonica; 95.5%, 1.3%, 3.1% in P. frutescens Britton var. acuta; 95.1%, 1.8%, 3.1% in l. japoincus; 91.4%, 3.5%, 5.1% in l. inflexus; 96.8%, 0.7%, 2.5% in l, serra; 96.0%, 1.8%, 2.2% in Mosla dianthera; 94.7%, 2.0%, 3.3% in M. punctulata; 90.1%, 2.4%, 7.5% in Nepeta cataria; 90.1%, 3.4%, 6.5% in Agastache rugosa; 86.3%, 3.3%, 10.4% in Elsholtzia ciliata; 94.3%, 1.5%, 4.3% in Salvia splendens; 87.2%, 2.9%, 9.0% in Lycopus maackianus; 87.0%, 1.5%, 11.5% in Clinopodium chinense var. parviflorum; 91.8%, 1.6%, 6.6%; 95.5%, 0.4%, 4.1% in Leonurus sibricus; 89.0%, 1.4%, 9.6% in Scutellaria baicalensis. 3) Total lipids revealed the predominace of unsaturated fatty acids (82.0-94.5%) and larger variations were found in the composition of ${\alpha}-linolenic$ acid (0.4-67.9%) and linoleic acid (11.2-82.9%). High level of ${\alpha}-linoenic$ acid was present in P. frutescens Britton var. japonica (67.9%), P. frutescens Britton var, acuta (66.0%), lsodon japonicus (65.2%), l. inflexus (59.0%), l. serra (57.3%), Mosla dianthera (60.9%), Nepeta cataria (58.3%), Agastache rugosa (58.5%) and Elsholtzia ciliata (46.2%), and followed by linoleic acid (11.2-32.1%) and oleic acid (9.3-12.2%). However, linoleic acid was the most predominant component in the total lipids of Clinopodium chinense var. parviflorum (62.4%), Ametystea caerules (82.9%), Leonurus sibricus (60.9%) and Scutellaria baicalensis (63.4%), with very small amounts of ${\alpha}-linolenic$ acid (0.4-3.1%). The total lipids of Salvia splendens, Lycopus maackianus and Mosla punctulata also contained linoleic acid of 31.3%, 48.8% and 53.4%, with a considerable amount of ${\alpha}-linolenic$ acid of 34.5% 27.0% and 16.7%. Palmitic acid was the major saturated fatty acid in all the oils investigated (4.1-14.2%). 4) Fatty acid profiles of neutral lipids bore a close resemblance to those of total lipids in all the seed oils, but different from those of glycolipids and phospholipids. Fatty acid composition pattern of glycolipids and phospholipids showed a considerably increased level of saturated fatty acids (19.0-66.8%, 17.8-35.2%) mainly composed of palmitic acid and stearic acid, and a noticeable low level of unsaturated fatty acids (41.2-80.9%, 64.7-82.1%) which was ascribed to the decrease in ${\alpha}-linolenic$ acid of high ${\alpha}-linolenic$ acid seed oils, and in linoleic acid of high linoleic seed oils, compared to that of total lipids and neutral lipids.

Toxin Produced by Pathogenic Vibrios Isolated from Sea Food (수산물에서 분리된 병원성 비브리오균의 용혈성독소)

  • CHANG Dong-Suck;SHINODA Sumio
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.27 no.2
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    • pp.107-113
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    • 1994
  • Among the currently recognized pathogenic vibrios, V. vulnificus and V. cholerae non O1 are the most serious bacteria from the point of view of sea food hygiene in Korea. In this paper, the authors compared the hemolytic activities of the crude hemolysin produced by V. vulnificus and V. cholerae non O1 isolated from shellfish collected in Chungmoo, Korea. The authors also attempted to improve the purification method of V. vulnificus hemolysin(VVH) and tried to make antiserum with the purified hemolysin. VVH was produced in abundance in heart infusion broth containing $2\%$ NaCl in a shaking cultivation process(140rpm) at $37^{\circ}C$ for 15 hours. While hemolysin production patterns of V. cholerae non O1 were quite different by the strain during the culture times compared with the V. vulnificus. Hemolytic activity of the VVH on sheep erythrocytes was stronger than those of rabbit, but hemolytic activities of the hemolysin produced by V. cholerae non O1 on rabbit erythrocytes were as much as twice as strong as on those of sheep and horse. VVH was purified by two steps of hydrophobic column chromatography on Phenyl-Sepharose HP with Fast Protein Liquid Chromatography(FPLC). Purification fold and yield of VVH was much improved by changing the elution buffer's pH from 6.0 to 9.8 and adding $1\%$ CHAPS(a zwitter ionic detergent) and $50\%$ ethylene glycol to the 10mM glycine buffer during the repeated hydrophobic column chromatography. Homogeneity of the purified hemolysin was shown by polyacrylamide gel electrophoresis. According to the five times repeated purification results, the specific activity was increased 27500 times and the yield was improved by $23.4\%$ on average. About $250{\mu}g$ of purified hemolysin was harvested from the 2400ml of culture supernatant of V. vulnificus. Molecular weight of VVH was estimated to be 50KDa by the SDS-PAGE and the neutralization scores of the obtained antiserum acting against VVH were $2000{\sim}8500$.

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Antioxidant activity and comparative analysis of major functional compounds in liqueur using coffee and coffee-ground (커피와 커피박 침출주의 항산화 활성 및 주요 생리활성 물질의 비교 분석)

  • Kang, Jeong Eun;Park, Seon Kyeong;Guo, Tian Jiao;Kang, Jin Yong;Lee, Du Sang;Kim, Jong Min;Kwon, O-Jun;Lee, Uk;Heo, Ho Jin
    • Food Science and Preservation
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    • v.23 no.4
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    • pp.560-567
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    • 2016
  • Sensory evaluation, in vitro antioxidant activities and main compounds of coffee water-extract, coffee liqueur (CL) and coffee-ground liqueur (CGL) were investigated to consider their industrialization. Sensory evaluation showed that all groups of CGL without 25% CGL (3 month) were relatively higher than CL groups. Total phenolic compounds and in vitro antioxidant activities such as 1,1-diphenyl-2picryl-hydrazyl (DPPH) radical scavenging activity and ferric reducing/antioxidant power (FRAP) were also performed. The group of 35% CGL had higher total phenolic compounds than others, and the result of DPPH radical scavenging activity was similar to that of total phenolic compounds. In addition, 35% CGL is comparable to the FRAP of coffee water extract (CE). Qualitative and quantitative analysis using high-performance liquid chromatography (HPLC) were performed, and chlorogenic acid as a ployphenolic compound and caffeine as a nonpolyphenolic compound were detected in all samples. Moreover, the HPLC analysis showed that CGLs contain a larger amounts of chlorogenic acid (difference of 0.3~10.5%) and also greater amounts of caffeine (difference of 10.0~18.2%) more then CE. Consequently, these results suggest that coffee-ground as coffee by-products could be used as commercially available food substances because of its physiological molecules remained.

Quality Standardization and Isoflavone Glycoside Research of in Buseoktae(Yeongju bean) Cheonggukjang for Business Use from Yeongju Bean (영주 부석태 청국장시료의 이소플라본 배당체 탐색과 청국장의 품질 표준화)

  • Choi, Eun-Young;Yu, Jin-Hyeon;An, Hui-Jeong
    • Culinary science and hospitality research
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    • v.22 no.2
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    • pp.13-28
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    • 2016
  • This study performed quantitative analysis of isoflavone glycoside contents on Buseoktae, Daewon, Wooram beans and cheonggukjang made of Buseoktae beans from the LC/MS/MS. Also, the experiment carried out by means of RSM(response surface methodology), which included 10 experimental points for the two independent variables addition(40, 55, 70 g) and time(2, 3, 4 min) from the beginning point to boil of cheonggukjang. These were optimized using a Face-centered central composite design. Daidzein contents were $212.16{\mu}g/mL$ in Buseoktae, $212.21{\mu}g/mL$ in daewon, $158.54{\mu}g/mL$ in wooram beans. Genistein contents were $318.84{\mu}g/mL$ in Buseoktae, $310.50{\mu}g/mL$ in daewon, $262.71{\mu}g/mL$ in wooram beans. Total isoflavone contents were $532.50{\mu}g/mL$ in Buseoktae, $524.19{\mu}g/mL$ in Daewon, $422.71{\mu}g/mL$ in Wooram beans. Isoflavone contents of Buseoktae and Daewon were quite similar, relatively contents of Wooram beans were low. Total isoflavone contents of Buseoktae cheonggukjang (for business use) was $430.10{\mu}g/mL$ in A ($32^{\circ}C$, 96 h fermentation), $460.09{\mu}g/mL$ in B ($36{\sim}40^{\circ}C$, 30 h fermentation), $417.46{\mu}g/mL$ in C cheonggukjang($36{\sim}38^{\circ}C$, 72 h fermentation), B cheonggukjang was just a bit more than A, C cheonggukjang. The estimated response surfaces confirmed that the amount and time had significant effects on taste. The optimum condition of Buseoktae cheonggukjang taste was predicted to be 55.20 g addition at 2.92 min.

Relationships between Fatty Acids and Tocopherols of Conventional and Genetically Modified Peanut Cultivars Grown in the United States (미국산 전통품종과 유전자 재조합 땅콩품종의 지방산과 토코페롤의 상관관계)

  • Shin, Eui-Cheol
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.42 no.10
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    • pp.1618-1628
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    • 2013
  • Relationships between fatty acids and tocopherols in conventional and genetically modified peanut cultivars were studied by gas chromatography with flame ion detector and high performance liquid chromatography with fluorescence detection. Eight fatty acids and four tocopherol isomers in the sample set were identified and quantified. Oleic acid and linoleic acid are major fatty acids and the ratio of oleic and linoleic acids ranged from 1.11 to 16.26. Tocopherols contents were 6.76 to 12.24 for ${\alpha}$-tocopherol (T), 0.08 to 0.39 for ${\beta}$-T, 5.28 to 15.02 for ${\gamma}$-T, and 0.17 to 1.17 mg/100 g for ${\delta}$-T. Correlation coefficient (r) for fatty acids and tocopherols indicated a strong inverse relationship between oleic & linoleic acids (r=-0.97, P<0.05) and positive relationships between palmitic & linoleic acids (r=0.95, P<0.05) and ${\gamma}$-T & ${\delta}$-T (r=0.83, P<0.05). Principal component analysis (PCA) of fatty acids and tocopherols gave four significant principal components (PCs, with eigenvalues>1), which together account for 85.49% of the total variance in the data set with PC1 and PC2 contributing 45.27% and 21.33% of the total variability, respectively. Eigen analysis of the correlation matrix loadings of the four significant PCs revealed that PC1 was mainly contributed by palmitic, oleic, linoleic, and gondoic acids, while PC2 was by behenic acid, ${\beta}$-T, and ${\gamma}$-T. The score plot generated by PC1-PC2 identified sample clusters in the two spatial planes based on the oleic and linoleic acids. The score plot PC3-PC4 didn't separate sample groups.

Quantitative Analysis for Components of Epimedium koreanum (음양곽 주성분의 정량분석)

  • Han, Yong-Nam;Hwang, Keum-Hee;Lee, Mie-Soon
    • Korean Journal of Food Science and Technology
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    • v.28 no.4
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    • pp.616-623
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    • 1996
  • Eum Yang Kwak, the aerial part of Epimedium koreanum, is widely used as a folk medicine for stimulant in man, tonic, and hypotensive purpose. The plant contains icariin (a specific flavonoid), magnoflorine (an alkaloid) and tannin, but their contents are not known until now. In this paper, a quantitative analysis method for them was developed. Determination of icariin and magnoflorine was successfully achived by high performance liquid chromatography equipped with a UV detector in the ranges of $0.1{\sim}0.4\;mg$ and $0.002{\sim}0.1\;mg\;per\;ml$ sample, respectively. Extraction of the plant was carried out with water or 50% ethanol using different decocting temperatures and times. Icariin was well extracted either by water ($100^{\circ}C$, 3hr) or 50% ethanol ($85^{\circ}C$, 1hr), and its content in the plant was measured to be 0.94%. On the other hand, magnoflorine was fully extracted by 50% ethanol ($85^{\circ}C$, 1hr), and its content was determined to be 0.16%. Therefore, decoction of the medicinal plant with water at $100^{\circ}C$ for 3hr turned out to be recommendable for the best extraction.

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Inhibitory Activities of Water Extracts of Black Ginseng on HCl/Ethanol-Induced Acute Gastritis through Anti-Oxidant Effect (흑삼 열수 추출물의 항산화 효과를 통한 염산/에탄올로 유발된 위염 억제 작용)

  • Kim, Min Yeong;Kwon, O Jun;Noh, Jeong Sook;Roh, Seong-Soo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.9
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    • pp.1249-1256
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    • 2016
  • Black ginseng (BG) obtained by a 9-fold steaming process of Panax ginseng has been reported to have anti-oxidative, anti-obesity, and anti-diabetes effects. The current study evaluated the protective effect of BG by steaming time in an HCl/ethanol-induced acute gastritis model. BG was divided into four samples according to steaming-drying processing (Gin1, Gin3, Gin6, and BG). High performance liquid chromatography analysis, free radical scavenging activity, and total phenol and flavonoid contents were examined in ginseng and four BG samples. Compared with ginseng, BG showed a stronger radical scavenging effect and higher contents of total phenol and flavonoids. To evaluate the anti-gastritic effect of BG, mice were distributed into five groups: normal mice (N), acute gastritic mice with distilled water (CON), acute gastritic mice with 100 mg/kg of ginseng (Gin0), acute gastritic mice with 100 mg/kg of BG (BG), and acute gastritic mice with 10 mg/kg of sucralfate (SC). After 1 hour of pre-treatment with water, extracts (Gin0 and BG), or drug (SC), experimental groups except for N were orally administered 0.5 mL of 150 mM HCl/60% ethanol (v/v) mixture. Blood was collected 1 hour later from the heart, and gastric tissue was harvested. Reactive oxygen species (ROS) levels were measured in serum, and related protein expression was examined by Western blot assay. In HCl/ethanol-induced acute gastritic mice, treatment with ginseng or BG improved mucosal damage in the histological evaluation. The serum ROS level significantly decreased in the BG-treated group compared with the CON group. Furthermore, expression of inflammatory cytokines significantly decreased in the BG-treated group compared with the CON group. Based on these results, antioxidant and anti-gastritic activities of ginseng were enhanced by streaming-drying processing, in part due to an increase in biological active compounds.

Antibacterial and Antimutagenic Effects of Sweetpotato Tips Extract (고구마 끝순 추출물의 항균 및 항돌연변이 효과)

  • Lee, Joon-Seol;Shin, Mee-Jin;Park, Yang-Kyun;Ahn, Young-Sup;Chung, Mi-Nam;Kim, Hag-Sin;Kim, Jeong-Mok
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.52 no.3
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    • pp.303-310
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    • 2007
  • Sweetpotato shoot tops (leaves, tips and petioles) are known to be very useful parts as vegetables because of their high nutritive values and great biomass yield. In this study, the phenolic compound contents, antibacterial activity, mutagenic activity, and antimutagenic activity were investigated in sweetpotato tips that were 10-15cm of shoot top including stems, petioles and tender leaves after sprout of storage roots. The study was done by extracting sweetpotato tips with 80% ethanol and the ethanol fraction was re-extracted with hexane, chloroform, ethyl acetate, butanol and water. In ethyl acetate and butanol fractions, total phenolic compounds contained 95. 6mg/g extract and 69.3 mg/g extract, respectively, The antibacterial activity was measured using the paper disk method with concentrations of 1, 2, 5 and 10 mg/disk of butanol and ethyl acetate fractions against L. monocytogenes and S. Typhimurium strains. Higher doses of solvent extracts showed the higher antibacterial activities. In addition, 5, 10 and 20 mg/mL of the extracts were tested to determine the antibacterial activity in liquid culture. The sweetpotato leaf extract by ethyl acetate showed 1 log reduction compared to control after 24 hrs on Listeria monocytogenes, but 20 mg/ml of butanol extract completely inhibited the growth of the pathogen after 12 hrs. The extracts from ethyl acetate or butanol on Salmonella Typhimurium did less than 1 log reduction during cultivation compared to control. The numbers of S. Typhimirium TA98 and TA100 revertant colonies were 29-33 and 159-188 CFU/plate, respectively, indicating that solvent extracts were no mutagenic activity. The antimutagenic test was performed by adding direct mutagen 2-NF and MMS, and butanol and ethyl acetate showed antimutagenic effect. Thus, this study showed that sweetpotato tips had high phenolic contents and both antimicrobiol and antimutagenic properties. Sweetpotato tips would be good nutritive source because of their high nutrient content without any toxicity in consuming.