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가속용매추출장치(ASE) 및 다층크로마토그래피를 이용한 어패류 중의 dioxin-like PCBs의 분석
서정혁(Jung-hyuck Suh),오금순(Keum-Soon Oh),박성수(Seongsoo Park),정소영(So-young Chung),소유섭(You-sub Sho),김정수(Jung-soo Kim),장승철(Seoung-chul Jang),이종옥(Jong-ok Lee),김희연(Hee-Yun Kim),우건조(Gun-jo Woo) 한국식품과학회 2007 한국식품과학회지 Vol.39 No.2
식품 중에서 dioxin-like PCBs를 분석하기 위하여 가속용매추출기를 이용하여 추출하고 다층컬럼크로마토그래피를 이용하여 정제하는 분석법을 확립하였으며 어패류에 실제로 적용하여 그 오염수준을 조사하였다. 시료는 균질화하여 33㎖ 추출 셀을 포함한 가속용매추출기를 이용하여 추출하였다. 추출액을 산성 실리카겔, 중성 실리카겔 및 염기성 실리카겔이 연속으로 충전된 컬럼을 통과하여 지방 및 방해성분을 제거하였다. 기기분석은 고 분해능 질량분석기를 이용하여 분해능 10,000에서 4 window MID (multiple ion detection) mode로 분석하였다. 분석결과 평균 회수율은 94.1-104.1%(±8.4)이었고 검출한계는 신호 대 잡음 비(S/N)>3에서 0.1 pg/g이었다. 확립된 분석법을 이용하여 식품시료에 적용한 결과 dioxin-like PCBs의 오염수준은 0.030-1.836 pg TEQ/g이었다. In this study, an analytical method was optimized for detecting dioxin-like PCBs in fish and shellfish. Here, homogenized samples were extracted using an accelerated solvent extraction (ASE) system with 33 ㎖ cell size. Multi-layer column chromatography, which consisted of acidic, basic, and neutral silica gels, was used for the clean up of the extracts. The instrumental analysis was executed by HRGC/HRMS to a resolution of 10,000 using 4 window multiple ion detection (MID) mode. For the results, the average recoveries ranged from 94.1 to 104.1% (±8.4) and the limit of detection was approximately 0.1 pg/g at S/N ratio >3. Finally, the detected concentrations of dioxin-like PCBs for fish and shellfish were in the range of 0.030-1.836 pg TEQ/g.
최훈 ( Hoon Choi ),김형수 ( Hyung Soo Kim ),서정혁 ( Jung Hyuck Suh ),백옥진 ( Ock Jin Paek ),강영운 ( Young Woon Kang ),이준구 ( Joon Goo Lee ),봉영훈 ( Young Hoon Bong ),곽지연 ( Ji Yeon Kwak ),이승일 ( Seung Il Lee ),신민홍 ( 한국환경농학회 2013 한국환경농학회 학술대회집 Vol.2013 No.-
This study was carried out to survey the levels of mercury in root vegetables and assess dietary exposure / risk to the Korean population health. Various samples including Panax ginseng C.A mayer, Codonopsis lanceolata, and Platycodon granditloum were collected from markets across Korea. The concentrations of mercury were measured using automatic mercury analyzer. The analytical and sampling methods in this study were full validated. The mercury content in root vegetables was determined below 100 μg/kg (maximum residue of mercury for salt established in Korea). For risk assessment, probable daily intake was calculated and compared with PTWI (tolerable weekly intake) established by JECFA. The level of overall exposure to mercury for Korean through root vegetables was below 1% of the recommended JECFA levels, indicating of little possibility of risk. Whereas, MFDS was conducted to assess the dietary exposure to mercury from food intake, based on several reports regarding mercury published by MFDS in the 2000s. The mean and 95th percentile for exposure to dietary mercury were 4.29 and 12.48 μg/day, corresponding to 13.6% and 39.7% of PTWI, respectively.
백옥진 ( Ock Jin Paek ),김형수 ( Hyung Soo Kim ),서정혁 ( Jung Hyuck Suh ),강영운 ( Young Woon Kang ),이준구 ( Joon Goo Lee ),봉영훈 ( Young Hoon Bong ),최훈 ( Hoon Choi ),곽지연 ( Ji Yeon Kwak ),이승일 ( Seung Il Lee ),박기훈 ( 한국환경농학회 2013 한국환경농학회 학술대회집 Vol.2013 No.-
Alternaria toxins haver been found to be natural food contaminants in grains, sunflowers seeds, and some visibly decayed fruits in many countries. Their natural occurrence in cereals has been reported in different countries. Several studies have reported the relevance of the this genus in crop. However, there are no studies on the method validation of alternaria toxin in cereals in our contry. A simple and sensitive analytical method based on HPLC with PDA and mobile phases using 0.1% phosphoric acid and acetonitrile was developed for simultaneous determination of alternaria toxins. A method validation for the determination of alternaria toxins in cereals was validated. In short, the method is as follows : A test portion of a sample is extracted with a mixture of methanol/water(90/10, v/v). This raw extract is then diluted, filtered, and applied to an SPE column. After washing and elution with acetonitrile, the elute is evaporated to dryness. After toxins in the dry residue in mobile phase are injected into a high performance liquid chromatography, and detected and quantified by PDA. For alternaria toxins in the cereals, Recovery test, calibration curves (Linearity), LOD and LOQ were successfully confirmed and Reproducibility relative standard deviations(RSDR) and Repeatability relative standard deviations(RSDr) for cereals samples were below 15% for the spiked cereals at 100 ug/kg. Since all these parameters lie well within the acceptable range set forth in EU mycotoxin method validation legislation. This method is The proposal method is sensitive, repeatable and rapid enough to apply to officially routine inspection of agricultural products including cereals.
허옥순,이재관,이정성,서정혁,주인선,허수정,김세은,김정근,신영희,유미자,김지연,심규창,김성환 식품의약품안전청 1998 식품의약품안전청 연보 Vol.2 No.-
신속 · 정밀하고 효율적인 짠류농약 검출을 위하여 극싱칼럼 (Extrelut-3')을 사옹한 SPE법을 시도하였다. 시료는 채소류체 사용하는 농약중 잔류성이 있고 식품공전상 시험 전처리가 각각 다른 Chlorothalonil등 6종의 농약을 선정하고 그들 표준액에 대한 PPIR수준의 농도로추출용라의 종류 및 용매량 등의 추출조건을 달리하여 회수율 등을 측정한 결과 최적의 분석조건을 얻었다. 1) 추출 용매량은 증가할수록 추출 수율이 높았고,용매 종류에 대한 추출수율은 각 농약별로 다소 차이는 있었으나 극성 정도가 비교적 높은 Ethyl acetate애서 평균 추출수율이 가장 높았다 2) 최대 평균회수율은 Ethyl acetate 60mL를 사웅할 경우로서 93.6%였다. 3)표준액을 시료에 첨가한 시험에서도 역시 Ethyl ace늘to가 푼출수율이 가장 높았으며 불순물 분리제거 효과도 LLE법 보다 월등히 우수하였다. 4) 각 농약별 검출한계는 치소 0.001ppin으로 농산물 중 미량 잔류하는 농약을 검출할 수 있을 것으로 사료된파. 그러므로 SPE법은 LLE법보다 경제적인 방법으로 판명되었으며, 앞으로 농산물 중 잔류농약 분석에서 LEE법을 대치할 쑤 있을 것으로 기대된다. Solid-phase extraction by polar column(Extrelut-3') was attempted to develope the fast and efficient method of detecting pesticide of farm product.5·ix kinds of pesticide used in farming fieldfrequently and different in pretreatment, were chosen from Korea Food Cord. Optfmal analysis condi-tions were determiBed from t31e recovery rate of standard pesticides according to extraction solvent andextraction volurae. Extraction yietd was increased as solvent polarity and extraction volume. Maximumrecovery rate was acquired at 93.6% when 60mL of ethyl acetate was used as eluent. Tllis method wasmore effective than liquid-liquid partition extract·ion method to eliminated the impurity and had 0.001ppm of detection limit. Therefore. solid-phase eEl=raction was expected to be economical substitute fortraditional liquid-liquid extT·action method.
원경풍,황인균,최동미,이강봉,오금순,서정혁,박성수,최영미,진영선,서동원,이은경,최수미 식품의약품안전청 2001 식품의약품안전청 연보 Vol.5 No.-
우리 국민이 일상의 식사를 통해 실제로 접취하는 농약의 양을 파악하기 위해 농약의 1일 섭취량 조사를 실시하였다. 패상식품은 국민건강 영양조사('98)를 글거로 농산물 및 육류, 어패류, 가공식픔 등 국민 다소비식풍 18개군 110종을 선정하여 전국 4개 도시(서울, 부샨, 대전, 광주1에서 구입하였으며 각각의 식품을 통상적인 방법에 파라 조리하여 동일식품별로 균일하게 혼합한 후 농약 잔류량을 분석하였다. 대상농약은 동시분석이 가능한 120종의 농약을 선택하여 BB-5 및 DB-17 c'apillary column을 이용, GC/ECD 및 GCJNPD로 분석한 후 CC/btSD로 확인하였다. 분꼭켤과 채소류 3건(오이, 토마토,껏잎) 및 과실류 1건(참외)에서 procymidone이 각각 0.073m9/kg, 0.03m9/kg, 1.149m9/kg, 0-065m9/ 검출되었으며, 그 꼭의 식품군에서는 농약이 검출되지 않았다 검출된 proc)rmidone의 1일 추정 섭취량 (EDI : Estimated Dail)· Intake)은 2.82#g/person/dat·이었으며, ADI와 비교하였을 패 0.05ff 이하로 안전성에는 문제가 없는 것으로 평가되만다 한편 비지방성 식품(쌀, 사과) 및 지방성 식픔(식용유)에 대한 븐석대상 농약들의 회수율은 70~120% 범위호 비교적 양호하였다. In order to estimate the intake of pesticide residues through food that is prepared to eat, Total Diet Study(TDS) was carried. The food Itst for the TDS was establishedthrough a nationwide food consumption survey('98) conducted by bfinistry of Health f: Welfare.Meats and their p~ffu(:Is, seafood fishes, processed foods as we31 as agricultural products vi'erepurchased at the grocery stores at 4 large cities(Seoul, Busan, Gwangju and Daejon) in Korea.The collected sampBes from 4 cities were treated in a similar cooking method that Ivas used a)honle and mixed into one sample. For this study, 120 pesticides con?monly anal?Fzed wereselected and the muBticlass multiresidue analIFsis methods for nonfatt? foods or fatt? foods deleanal!7zed bIF GC/ECD and NFD with DB-S and DB-17 capillary column and confirmed b!'eC/LISD. As a resu.It, procymidone fFas detected in three of vegetables and one offriuts(cucumber, tomato, perilla leaf and Korean melon) )t·ith 0.073re'k9, 0.030n1a/kg, 1.149m9/kgand 0.06ima#'kg. respectivelIT. These values were corresponded to 2.8f#8/person/da? of It)eestimated dail? intake(TDI). Comparing u·ith acceptable dailt'intake(.tDl). EDI w3s bolo)u0.oj% of .tDf. Recoveries o( IfO pesticides foFtifled In rice, apple and so?bean oil Ivere rangedfrom TO to 120%.