• 한국식품위생안전성학회지
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• 제37권1호
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• pp.1-8
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• 2022

본 연구는 2021년 2월부터 7월까지 잡곡 106건을 수거하여 잔류농약 실태조사를 하였다. 대형, 중소형 및 온라인 유통매장을 중심으로 국내 잡곡 40건과 수입 잡곡 66건을 수거하였고, GC/MSMS, GC/ECD, GC/NPD, LC/MSMS, UPLC/PDA, HPLC/FLD를 이용하여 다종농약 다성분분석법으로 잔류농약 341종을 분석하였다. 잔류농약이 검출된 잡곡은 대형유통매장 1건, 중소형 유통매장 2건, 온라인 유통매장 5건으로 총 8건(7.5%)이었고, 5건(4.7%)에서는 농약잔류허용기준을 초과하였다. 이들 잡곡에서는 MGK-264, chlorpyrifos, thiamethoxam, malathion, piperonyl butoxide, pirimiphos-methyl 등 6종의 농약 성분이 검출되었다. 검출된 잡곡은 강낭콩(1건), 녹두(6건), 수수(1건)이다. 검출된 잡곡 중 농약잔류허용기준을 초과한 품목은 수입 녹두(5건)로 미얀마산이었고, 초과한 농약 성분은 thiamethoxam이었다.

• 한국환경보건학회지
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• 제44권5호
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• pp.444-451
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• 2018

Objectives: This study was carried out to provide safe seafood to the public through simultaneous analysis rapid inspections for residual veterinary drugs in 150 fishery products in 2016. Methods: Quinolones (9), Sulfonamides (14), Penicillins (2), Cephalosporins (3), Tetracyclines (4), Macrolides (4), Lincosamides (2), Pleuromutilin (1), Phenicols (4), benzylpyrimidines (2), Others (1) Malachite green (2), and Melamine (1) were analyzed for 49 species using by HPLC and HPLC-MSMS. Results: There were six unsuitable samples, five among fish and one for crustaceans. Within the standard detection were five fish. The antibiotics found were Quinolones (50%), Tetracyclines (33%) and Penicillins (17%). Conclusions: As a result of the experiment, there were six unsuitable samples, five for fish and one for crustaceans. The most prevalent antibiotics were Quinolones. The quinolone antibiotics are highly persistent in fish tissues, so they require more time than the withdrawal period for other common veterinary drugs. Careful attention is required when they are used in fish farms.

• 한국동물위생학회지
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• 제32권3호
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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.

• Bulletin of the Korean Chemical Society
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• 제27권2호
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• pp.291-294
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• 2006

A highly sensitive high-performance liquid chromatographic-tandem mass spectrometric method (HPLC-MSMS) has been developed to quantify itraconazole in human plasma for the purpose of pharmacokinetic studies. Sample preparation was carried out by liquid-liquid extraction using loratadine as an internal standard. Chromatographic separation used a YMC $C_{18}$ column, giving an extremely fast total run time of 3 min. The method was validated and used for the bioequivalence study of itraconazole tablets in healthy male volunteers (n = 31). The lower limit of detection proved to be 0.2 ng /mL for itraconazole.

• 한국환경농학회지
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• 제39권2호
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• pp.122-129
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• 2020

BACKGROUND: Dissipation patterns of insecticides (acequinocyl, clothianidin, diflubenzuron, thiacloprid, and thiamethoxam) on strawberry grown in plastic-covered greenhouse were evaluated at 7 intervals including the preharvest interval after application. This study was performed to determine the residue concentrations, half-lives and dissipation rates in strawberry for the harvest periods. METHODS AND RESULTS: Acequinocyl, clothianidin, diflubenzuron, thiacloprid, and thiamethoxam were applied in accordance with critical good agricultural practices for strawberry. Strawberry samples were collected at 0, 1, 2, 3, 5, 7 and 10 days after application. Quantitaion was performed by HPLC/DAD and HPLC-MSMS system with C₁₈ column. The limit of quantitation (LOQ) values varied between were 0.00025~0.05 mg/kg on strawberry. The recoveries of acequinocyl, clothianidin, diflubenzuron, thiacloprid and thiamethoxam at two concentrations ranged from 70.9~104.9% on strawberry. The half-lives of pesticide dissipation on strawberry for two fields ranged from 1.3~8.2 days. The dissipation rates were evaluated according to the statistics method with a 95% confidence. CONCLUSION: The residue levels of insecticides (acequinocyl, clothianidin, diflubenzuron, thiacloprid, and thiamethoxam) on strawberry at 0-day after application were below the specified values by Korean MRL. To estimate dissipation rate constant of pesticides on crop for harvest periods, it is important to set the pre-harvest residue limit for human health and consumer protection in Korea.

• 농약과학회지
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• 제12권4호
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• pp.323-334
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• 2008

본 연구는 국내의 지리적표시제 등록특산물을 대상으로 농약 잔류실태를 조사하여 식품안전 정책수립의 기초자료와 잔류농약에 대한 식품의 안전성을 평가하고자, 지리적 표시 등록 특산물 17품목(마늘 1, 마늘 2, 마늘 3, 마늘 4,고추, 양파 1, 양파 2, 쌀 1, 쌀 2, 쌀 3, 참외, 사과, 밤, 대추, 황기, 표고버섯, 구기자)을 선정하여 잔류 실태를 조사하였다. 조사대상 농약으로는 다성분 분석농약 204종과 단성분 분석농약 5종(acephate, methamidophos, monocrotophos, omethoate, vamidothion)을 포함한 209종의 농약에 대해 잔류량을 조사하였으며, 분석장비로는 GC/MSMS, HPLC/UVD(PDA)와 GC/FPD를 사용하였다. 분석법방법으로는 식품공전의 83번 다성분분석법과 단성분분석법을 사용하였다. 분석결과 특산물 17품목 중 8품목(고추, 양파 1, 쌀 2, 쌀 3, 참외, 사과, 대추, 구기자)에서 잔류농약이 검출되었고, 검출시료수는 302건중 40건으로 13.2%의 잔류농약 검출율을 보였다. 그러나 모두 식품의 농약잔류허용기준 미만이었다.

• 대한화장품학회지
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• 제34권3호
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• pp.157-165
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• 2008

이전 연구에서 저자들은 나문재 추출물의 항산화 작용과 추출물 함유 크림의 유화 안정성에 대한 결과를 보고한 바 있다[1,2]. 본 연구에서는 thin layer chromatography(TLC), high performance liquid chromatography (HPLC)와 liquid chromatography/Electrospray Tandem mass spectrometry (LC/ESI/MS/MS), $^1H$-NMR을 이용하여 나문재 추출물에 대한 성분 분석을 수행하였다. 나문재 추출물 중 ethyl acetate분획의 TLC는 5개의 띠($SA1{\sim}SA5$)로 분리되었다. Ethyl acetate 분획의 당 제거반응 후 얻어진 aglycone 분획에 대한 HPLC 크로마토그램은 2개의 피이크(SAA 2 및 SAA 1)를 나타냈고, 각각 그 용리 순서는 quercetin, kaempferol이었으며 조성비는 quercetin 16.88%, kaempferol 83.12%로 kaempferol의 함량이 큰 것으로 나타났다. 또한 LC/ESI-MS/MS를 통해서 SA 2는 kaempferol-3-O-gluco-side로 SA 3는 quercetin-e-O-glucoside, SA 4는 kaempferol-3-O-rutinoside, SA 5는 quercetin-3-O-rutinoside로 확인되었다. LC/ESI-MS/MS의 스펙트럼에서 SAA 1은 탈양성자화된 aglycone 분획에 상용하는 분자이온 $[M-H]^$-(m/z285) 피이크를 나타냈으며, $^1$v 분석을 실시한 결과 [${\delta}$ 6.19 (1H, d, J=1.8Hz, H-6), ${\delta}$ 6.44 (1H, d, J=1.8Hz, H-8), ${\delta}$ 6.92 (2H, d, J=9.0Hz, H-3',5'), ${\delta}$ 8.04 (2H, d, J=9.0Hz, H-2',6')]에서 피이크들이 나타났다. 따라서 SAA 1은 kaempferol임이 확인되었다. SAA 2는 aglycone 분획에 상응하는 분자이온 $[M-H]^-$ (m/z 301)을 생성하였고, $^1H$-NMR 스펙트럼은 [${\delta}$ 6.20 (1H, d, J=2.0Hz, H-6), ${\delta}$ 6.42 (1H, d, J=2.0Hz, H-8), ${\delta}$ 6.90 (1H, d, J=8.6Hz, H-5'), ${\delta}$ 7.55 (1H, dd, J=8.6, 2.2Hz, H-6'), ${\delta}$ 7.69 (1H, d, J=2.2Hz, H-2')]에서 피이크들을 나타냈고, 따라서 SAA 2는 quercetin으로 확인되었다. 결론적으로, 이미 보고된 나문재 추출물의 항산화 작용 그리고 안정성 실험과 더불어 나문재 추출물의 성분분석은 새로운 기능성 화장품원료로서 응용이 가능함을 시사한다.