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Determination of Post-harvest Fungicide in Citrus Fruits Using LC-MS (LC-MS를 이용한 감귤류의 수확 후 처리 살균제 분석)

  • Choi, Su-Jeong;Kim, Eun-Jeong;Lee, Jae-In;Cho, In-Soon;Park, Won-Hee;Hwang, In-Sook;Kim, Moo-Sang;Kim, Gun-Hee
    • Korean Journal of Food Science and Technology
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    • v.45 no.4
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    • pp.409-415
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    • 2013
  • Post-harvest fungicide residue was measured in citrus fruits. Samples were collected from local markets in Seoul and analyzed using liquid chromatography coupled with mass spectrometry (LC-MS). LC-MS results were validated for the assay of pesticides by using linearity, accuracy, precision, and limits of detection and quantification. The linearity in the concentration ranged from 0.005 to 2.0 mg/kg ($R^2$ >0.999). Sample recoveries ranged from 80.2 to 98.3% with relative standard deviations below 4.0% for spiking levels from 0.01 to 1.0 mg/kg. The limits of detection ranged between 0.002 and 0.008 mg/kg, and the limits of quantification ranged between 0.006 and 0.027 mg/kg. The highest residue levels for carbendazim, thiabendazole, imazalil, and azoxystrobin in citrus fruits were 0.541, 0.958, 0.721, and 0.052 mg/kg, respectively. The pesticide residues found in citrus fruits were blow maximum residue limits (MRLs) and are not a serious public health problem.

ICP-MS와 MA-2를 이용한 버섯류 유해 중금속 모니터링

  • Han, Chang-Ho;Hwang, Gwang-Ho;Ko, Suk-Kyung;Kim, Soo-Jin;Kim, Hee-Soon;Kim, Yoo-Kyung;Park, Gun-Young;Kim, Dong-Yoon;Lim, Sang-Chul;Choi, Byung-Hyun;Kim, Min-Young
    • 한국약용작물학회:학술대회논문집
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    • 2010.10a
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    • pp.381-381
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    • 2010
  • 2010년 5월 중 서울 약령시와 서울시내 대형마트에서 유통 중인 약용버섯 및 식용버섯류 16품목 92건 대상으로 중금속(비소, 카드뮴, 납, 수은) 모니터링을 실시하였다. 식품의약품안전청에서 고시한 생약의 잔류오염물질 허용기준 및 시험방법에 따라 실험하였으며, 유통 버섯류의 중금속 함유실태를 파악하고, 버섯의 안전성 기준 제정을 위한 기초 자료를 제공하고자 본 실험을 실시하였다. 새송이버섯 등 생버섯 7종 15건에 대한 중금속 검사 결과 비소 0.01~0.26 mg/kg, 카드뮴 0~0.10 mg/kg, 납 0~0.03 mg/kg, 수은 0~0.007 mg/kg 으로 중금속 함유량이 낮았다. 상황버섯 등 11종 77건의 건조되어 식용 및 약용으로 사용되는 버섯류 중 노루궁뎅이버섯은 4건 중 2건(50.0 %)에서 카드뮴이 0.32~0.82 mg/kg으로 한약재 기준 대비 높게 검출되었으며, 상황버섯은 15건 중 5건(33 %)에서 카드뮴 0.58~0.85 mg/kg, 표고버섯은 9건 중 3건에서 카드뮴 0.42~0.74 mg/kg, 운지버섯 5건 중 1건(20.0 %)에서 1.66 mg/kg, 영지버섯 16건 중 2건(12.5%)에서 수은 0.415 mg/kg과 카드뮴 0.66 mg/kg이 분석되었다. 특히 아가리쿠스버섯은 10건 중 10건(100.0 %)에서 카드뮴(10건) 1.49~7.35 mg/kg, 수은(9건) 0.202~0.505 mg/kg으로 높은 유해중금속 함유량을 보이는 것으로 조사되었다.

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Mornitoring of non-steroidal anti-inflammatory drugs in livestock products (축산식품 중 비스테로이드성 항염증 약물의 잔류함량 모니터링)

  • Choi, Yoon-Hwa;Kim, Yoen-Joo;Shin, Bang-Woo;Lee, Jung-Hark
    • Korean Journal of Veterinary Service
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    • v.34 no.3
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    • pp.285-289
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    • 2011
  • This study was conducted to determine the content of non-steroidal anti-inflammatory drugs (NSAIDs) in meats available on the Korean markets. The analysis was carried out using following conditions; C18 column ($100{\times}2.1$ mm, 1.7 ${\mu}m$), mobile phase composed of DW (containing 0.1% formic acid): acetonitrile (containing 0.1% formic acid), binary pump at a flow rate of 0.3 ml/min and 5 ${\mu}l$ of injection volume, MS/MS detector with ESI positive mode. The calibration range of five NSAIDs showed linearity ($r^2{\geq}0.99$) at concentration range of 3.125~200 ${\mu}g$/kg. The recoveries in fortified muscle more than 78.7~100.3%. The detection limits for meloxicam, ketoprofen, flunixin, carprofen and tolfenamic acid were 3.5, 1.6, 1.7, 9.8 and 4.8 ${\mu}g$/kg, respectively. We also monitored NSAIDs residue in cattle muscle 51 samples. The test results, NSAIDs were all not founded.

Migration Measurement of Volatile Organic Compounds (VOCs) from Polystyrene-made Food Containers into Distilled Water (폴리스티렌 식품용기로부터 증류수로 용출되는 휘발성유기화합물의 분석)

  • Kim, Nam-Hoon;Kim, Ae-Kyeong;Cho, Tae-Hee;Park, Kyung-Ai;Kwak, Jae-Eun;Kim, Ji-Young;Kim, Il-Young;Chae, Young-Joo;Kim, Min-Young
    • Journal of Food Hygiene and Safety
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    • v.25 no.3
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    • pp.203-208
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    • 2010
  • In this study, the level of migration of 5 kinds of volatile organic compounds (VOCs) (toluene, styrene, ethylbenzene, isopropylbenzene and n-propylbenzene) into distilled water from polystyrene-made food containers was measured using Purge&Trap combined with GC/FID. The contents of the VOCs which have regulatory limits in Korea food code only for material specification were determined under three exposure conditions which were 30 min at $60^{\circ}C$, 30 min at $95^{\circ}C$ and actual situation of instant noodle intake. The calibration curve of 5 compounds showed good linearity ($^r2$ = 0.9976~0.9995) within the concentration range of 1~50 ng/mL. The limit of detection (LOD) and limit of quantification (LOQ) were validated at range of 0.041~0.092 and 0.135~0.304 ng/mL, respectively. The average migration contents of 5 compounds were below 5 ng/mL except for styrene. The average contents of styrene were highly detected at $95^{\circ}C$ for 30 min exposure (52.71 ng/mL). Under actual condition at instant noodle intake, the average contents of styrene was 17.23 ng/mL. The results demonstrated that the migration rate of VOCs was related to storage temperature and time.

The Content of Heavy Metals in Herbal Pills Used as General Processed Food and Risk Assessment of Heavy Metal Intakes (유통 환(丸)제품의 중금속 함량 및 위해성 평가)

  • Kim, Sung-Dan;Jung, Sun-Ok;Kim, Bog-Soon;Yun, Eun-Sun;Chang, Min-Su;Park, Young-Ae;Lee, Young-Chul;Chae, Young-Zoo;Kim, Min-Young
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.39 no.7
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    • pp.1038-1048
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    • 2010
  • The purpose of this study was to investigate some heavy metals (Pb, Cd, Cr, Cu, Hg) in 52 commercial herbal pills used as general processed food, to identify weekly heavy metal intakes from herbal pills and to evaluate their potential health risks. The samples were digested with a microwave and determinations of heavy metal residues were carried out by inductively coupled plasma mass spectrometry (ICP-MS) and mercury analyzer. The mean values of heavy metal contents for herbal pills used as general processed food were Pb 0.421 (0.032~1.630), Cd 0.157 (0.011~0.515), Cr 1.033 (0.112~9.933), Cu 6.923 (1.333~16.755), Hg 0.010 (0.001~0.088) mg/kg. Lead contents of herba and cadmium of algae, herba were high (ANOVA-test, p<0.05). Levels of cadmium concentrations exceeding WHO reference values (0.3 mg/kg) were observed in 10 samples (4 species). The significant correlation was observed between Pb and Cd (r=0.633, p<0.01). The weekly intakes of Pb, Cd, Cr, Cu, Hg from herbal pills were 1.112 (0.072~5.088), 1.614 (0.029~9.257), 3.000 (0.252~23.690), 0.182 (0.008~1.235), 0.220 (0.000~0.420)%, respectively, as compared with the Provisional Tolerable Weekly Intake (PTWI) established by Joint FAO/WHO Expert Committee for food safety evaluation. Our data suggest regulations limiting heavy metals in herbal pills used as general processed food.

ABT-737 ameliorates docetaxel resistance in triple negative breast cancer cell line

  • Hwang, Eunjoo;Hwang, Seong-Hye;Kim, Jongjin;Park, Jin Hyun;Oh, Sohee;Kim, Young A;Hwang, Ki-Tae
    • Annals of Surgical Treatment and Research
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    • v.95 no.5
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    • pp.240-248
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    • 2018
  • Purpose: This study aimed to validate the synergistic effect of ABT-737 on docetaxel using MDA-MB-231, a triple negative breast cancer (TNBC) cell line overexpressing B-cell lymphoma-2 (Bcl-2). Methods: Western blot analysis was performed to assess expression levels of Bcl-2 family proteins and caspase-related molecules. Cell viability was assessed by 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay. Cell cycle distribution was determined by flow cytometry analysis. Benzyloxycarbonyl-Val-Ala-Asp(OMe)-fluoromethylketone (z-VAD-fmk) was used for pretreatment to assess the role of caspases. Results: Cell viability of MDA-MB-231 after combination treatment with ABT-737 and docetaxel was significantly lower than that after docetaxel or ABT-737 monotherapy based on MTT assay (both P < 0.001), with a combination index of 0.41. The proportion of sub-G1 population after combination treatment was significantly higher than that after docetaxel or ABT-737 monotherapy (P = 0.001, P = 0.003, respectively). Pretreatment with z-VAD-fmk completely restored cell viability of MDA-MB-231 from apoptotic cell death induced by combination therapy (P = 0.001). Although pro-caspase-8 or Bid did not show significant change in expression level, pro-casepase-9 showed significantly decreased expression after combination treatment. Cleaved caspase-3 showed increased expression while poly (ADP-ribose) polymerase cleavage was induced after combination treatment. However, hypoxia-inducible factor 1-alpha and aldehyde dehydrogenase 1 totally lost their expression after combination treatment. Conclusion: Combination of ABT-737 with docetaxel elicits synergistic therapeutic effect on MDA-MB-231, a TNBC cell line overexpressing Bcl-2, mainly by activating the intrinsic pathway of apoptosis. Therefore, adjunct of ABT-737 to docetaxel might be a new therapeutic option to overcome docetaxel resistance of TNBCs overexpressing Bcl-2.

Determination and survey of fluoroquinolones in meats and eggs (II) (식육 및 계란에서 플루오로퀴놀론계 항균물질 정량분석 및 잔류조사 (II))

  • Choi, Yoon-Hwa;Kim, Yeon-Ju;Lee, Kyung-Hye;Kang, Young-Il;Lee, Jung-Hark
    • Korean Journal of Veterinary Service
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    • v.32 no.3
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    • pp.281-286
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    • 2009
  • Fluoroquinolones in muscle and egg were separated by liquid extraction and determined. The analysis was carried out using following conditions; C18 column ($150{\times}4.6mm$, $5{\mu}m$), mobile phase composed of D.W. (containing 0.4% triethylamine and phosphoric acid) : methanol : acetonitrile (780:100:120, v/v/v), quarternary pump at a flow rate of 0.9ml/min and $20{\mu}l$ of injection volume, fluorescence detector with EX 278nm/Em 456nm. The calibration range of seven fluoroquinolones showed linearity ($r^2{\geq}0.999$) at concentration range of $0.025{\sim}0.8{\mu}g/ml$. The recoveries in fortified muscle and egg represented more than 81.3%. The detection limits for ofloxacin, norfloxacin, ciprofloxacin, enrofloxacin, danofloxacin, saraloxacin and orbifloxacin were 3.1, 2.5, 3.6, 1.7, 0.9, 2.5 and $2.1{\mu}g/kg$, respectively. We also monitored fluoroquinolones residue in the sample (chicken muscle 182, cattle muscle 140, pig muscle 139, egg 212) using EEC-plate (E. coli ATCC 11303) screening and HPLC confirmation methods. The screening test results, fluoroquinolones, antibacterial substances were all negative.

Analysis of Hexaconazole in Agricultural Products using Multi Class Pesticide Multiresidue Method (다종 농약 다성분 분석법을 이용한 농산물 중 hexaconzole 분석)

  • Choi, Su Jeong;Hwang, In Sook;Cho, Tae Hee;Lee, Jae In;Lee, In Sook;Yook, Dong Hyun;Park, Won Hee;Kim, Moo Sang;Kim, Gun Hee
    • Journal of Food Hygiene and Safety
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    • v.30 no.4
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    • pp.366-371
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    • 2015
  • This work was conducted to apply the multi class pesticide multiresidue method for determining the use of hexaconazole in the agricultural products using GC-NPD. The multi class pesticide multiresidue method results were validated for the assay of hexaconazole by using linearity, accuracy, precision, limit of detection and quantitation. The linearity in the concentration ranged from 0.025 to 5.0 mg/L ($R^2$ > 0.999). Lettuce recoveries ranged from 89.42% to 94.15% with relative standard deviations below 7.78%, for spiking levels from 0.04 to 4.0 mg/kg. The limit of detection was 0.04 mg/kg, and the limit of quantitation was 0.11 mg/kg. The intra- and inter-day precisions were 2.42~3.49% and 4.90~7.78%, respectively. We suggested that the multi class pesticide multiresidue method for determining hexaconazole was highly accurate and reproducible, and it will be used as a routine analysis in agricultural products.

Survey of the heavy metal contents in avian eggs from Korean markets (국내 유통 중인 식용란의 중금속 함량 조사)

  • Kang, Kyoung-Sook;Park, Hyoung-Sook;Choi, Tae-Seok;Shin, Bang-Woo;Lee, Jeong-Hark
    • Korean Journal of Veterinary Service
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    • v.34 no.3
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    • pp.279-284
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    • 2011
  • This study was carried out to estimate the heavy metal contents (Pb, Cd, Cr, Cu, Mn) in avian eggs sold in Seoul area, Korea from August to December, 2010. The contents of lead, cadmium, chrome, copper, manganese were estimated by inductively coupled plasma mass spectrometry. The concentrations of heavy metals (mean${\pm}$standard deviation, mg/kg) in the avian eggs were as follows: Pb $0.010{\pm}0.018$, Cd $0.000{\pm}0.001$, Cr $0.018{\pm}0.022$, Cu $0.637{\pm}0.163$, Mn $0.397{\pm}0.132$. The contents of lead and cadmium in the eggs were lower than that in meat and other foods of previously reported results. Whereas the contents of copper, manganese were similar to the previously previous results. The average daily intakes of lead and cadmium in the avian eggs were 0.1 and 0.8% respectively, as compared with PTWI (Provisional Tolerable Weekly Intakes) established by FAO/WHO Expert Committee for Food Safety Evaluation.

The Evaluation on the Pollution Level of Playgrounds for Children in Seoul Metropolitan (서울시내 어린이 놀이터 토양오염도 평가)

  • Lee, Jun-Bok;Kim, Gyeo-Bung;Jung, Kweon;Kim, Min-Young
    • Journal of Environmental Health Sciences
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    • v.32 no.4 s.91
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    • pp.249-253
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    • 2006
  • This survey study was performed to evaluate the pollution level of playgrounds for children at 49 different sampling sites in Seoul metropolitan. Results were as follows. 1. Soil pH ranged from 6.0 to 9.2. 2. Average concentrations of heavy metals were 0.101 mg/kg of Cd, 4.470 mg/kg of Cu, 0.10 mg/kg of As, 5.35 mg/kg of Pb, 0.017 mg/kg of $Cr^{6+}$ 0.0051 mg/kg of Hg, which were lower than Korean soil precaution level. 3. The SPCs of all areas were below 100, which is 1st grade. In conclusion, the pollution level of playgrounds for children was safe.