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HRGC/HRMS를 이용한 국내유통 육류 중 다이옥신류 분석
최동미,허수정,정지윤,원경풍,Choi, Dongmi,Hu, Soojung,Jeong, Jiyoon,Won, Kyungpoong 한국분석과학회 2001 분석과학 Vol.14 No.1
식품 중에 미량 존재하는 다이옥신류를 분석하기 위하여 육류인 소고기 돼지고기 닭고기를 서울 춘천 대전 광주 부산의 5대 도시 시장 등에서 채취하여 HRGC/HRMS를 이용한 동위원소희석법으로 분석하였다. 시료를 균질화하여 Soxhlet 추출 후 지방함량을 측정하고 정제를 하여 dioxin 7종, furan 10종 및 co-planar PCB 3종에 대하여 HRGC/HRMS로 분리능 10,000에서 분석하였다. 각각의 congener에 대한 회수율은 80-153%이었으며, 검출한계는 congener에 따라 차이는 있었으나 S/N>3에서 0,01ppt 수준이었다. 대상시료의 검출량을 WHO-TEF에 의한 TEQ로 산출한 결과 다이옥신의 평균잔류수준은 소고기 0.018, 돼지고기 0.008, 닭고기 <0.001 pgTEQ/g이었으며, non-ortho co-planar PCBs의 평균잔류수준은 소고기 0.008, 돼지고기 0.002, 닭고기 0.001 pgTEQ/g으로 닭고기의 오염수준이 제일 낮게 나타났다. 또한 분석시료에서 다이옥신류의 분포패턴을 살펴보면 OCDD의 비율이 상대적으로 높게 나타났으며, co-planar PCBs의 경우는 77번의 비율이 상대적으로 높게 나타났다. To measure the levels of dioxins in food selling at local markets, meat was analyzed by high resolution gas chromatography/high resolution ass spectrometry (HRGC/HRMS). The food samples were obtained from 5 large cities of Seoul, Chunchon, Daejon, Kwangju and Busan in Korea. All the samples were minced and extracted with Soxhlet extractor for 18 hours. After extraction, extracts were cleaned up by sulfuric acid impregnated silica gel, purified on a series of silica gel, alumina, carbon column chromatography and then analyzed by HRGC/HRMS. The contaminated levels were calculated as the TEQs by multiplying with the corresponding WHO-TEFs for each congeners. The overall recoveries were ranged from 80% to 153% and the limit of detection was about 0.01 ppt at S/N>3. The levels of PCDD/Fs for beef, pork and chicken were 0.018, 0.008 and <0.001 pgTEQ/g, respectively. In addition, the levels of non-ortho-co-planar PCBs for beef, pork and chicken were 0.008, 0.002 and 0.001 pgTEQ/g, respectively. Among food samples analyzed, chicken showed the lowest level of dioxin-like compounds. Regarding congener pattern, OCDD and PCB #77 were the highest contributing congeners.
Headspace-GC/MS를 이용한 음료 중 벤젠 분석
최동미,김은주,박상애 한국식품위생안전성학회 2007 한국식품위생안전성학회지 Vol.22 No.4
A selective analytical method of headspace-GC/MS has been applied to determine levels of ben-zene in beverages. Food samples were 85 including 2 fruit juices, 6 fruit beverages, 11 carbonated beverages, 5mixed beverages, and 4 beverage concentrations, and 7 extracted beverages. For phase equilibration of headspace,sample was stirred at 40oC for 30 min. The oven temperature was 60oC and elevated to 180oC at 15 oC/min. The inter-nal standard was benzene-d6. The identification was done by the selected target ions such as m/z 51, 77, and 78 andthe confirmation was done by the response ratio of m/z 77 to m/z 78 between sample and standard. The overall recov-eries were ranged from 91% to 101% and the limit of quantification was 1 g/kg. The average level of benzene were5 g/kg for fruit beverages, 2 g/kg for mixed beverages and 7 g/kg for extractedbeverages.
최동미,정지윤,장문익,임무혁,박건상,홍무기 한국분석과학회 2005 분석과학 Vol.18 No.3
A selective method of high performance liquid chromatography with UV detector has been applied to determine 4 tetracycline antibiotics in the animal food, simultaneously. The targets were chlortetracycline (CTC), doxycycline (DC), oxytetracycline (OTC), and tetracycline (TC) that are used routinely in veterinary medicine for prevention and control of disease. Food samples were beef, pork, chicken, milk, whole egg, flatfish (Limanda yokohamae), jacopever (Sebastes hubbsi), seabream (Chrysophrys major), eel (Anguilla japonica) and lobster (Hommarus americanus). After extracting food samples with 20% trichloroacetic acid and McIlvaine buffer, they were purified by a C18 SPE cartridge with 0.01M methanolic oxalic acid solution. The concentrated residue was re-dissolved in methanol, filtered, cleaned up and analyzed on a C18 column. The mobile phase was a mixture of 0.01M oxalic acid and acetonitrile with a gradient ratio from 85:15 to 60:40. The UV wavelength was 365nm. The overall recoveries were ranged from 71% to 98% and the limit of detections were 0.022 for CTC, 0.012 for DC and OTC and 0.009 mg/kg for TC at signal/noise > 3, respectively. As results, CTC, DC and TC were not detected in all selected food samples, however, OTC was detected in meat and fishes. The determined level of OTC was 0.04ppm for pork, 0.17ppm for flatfish and 0.05 and 0.08ppm for jacopever, that were within the Maximum Residue Limits (MRLs) in the food.