• 분석과학
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• 제19권5호
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• pp.415-421
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• 2006

채소류 및 과일류 중 PAHs 분석방법을 확립하고 오염실태 파악을 위하여 서울, 춘천, 대전, 광주, 부산의 5대 도시 시장에서 채소류 13종, 과일류 5종 총 210건을 채취하였다. 균질화된 시료를 dichloromethane으로 초음파추출하고 탈수한 후 Sep-Pak Florisil Cartridge로 정제하여 HPLC/FLD로 동시 정량 분석하였다. 시료에 표준물질을 spike하여 전처리 후 기기분석한 결과, 각각의 PAH에 대한 회수율은 약 95~102%였으며, 검출한계는 PAH에 따라 차이는 있으나 0.002~0.5 ng/g 수준이었다. 채소류 및 과일류 중 8가지 총 PAHs의 평균 함량은 0.19 ng/g이었으며 개별 평균 PAH 함량은 benzo(a)anthracene 불검출, chrysene 0.014 ng/g, benzo(b)fluoranthene 0.031 ng/g, benzo(k)fluoranthene 0.016 ng/g, benzo(a)pyrene 0.019 ng/g, dibenzo(a,h)anthracene 0.091 ng/g, benzo(g,h,i)perylene 0.016 ng/g, indeno(1,2,3-c,d)pyrene 불검출 수준이었다.

• 분석과학
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• 제22권1호
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• pp.109-117
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• 2009

조리 어패류 중 8종의 PAHs 실태파악을 위하여 어류 168건, 패류 40건을 분석하였다. 시료를 알칼리분해하여 n-hexane으로 추출하고 세척한 후 Sep-Pak Florisil Cartridge로 정제하여 HPLC/FLD로 정량 분석하였다. 각각의 PAHs에 대한 회수율은 약 88~112%였다. 조리어류에서 개별 PAH 평균 농도는 benzo(a)anthracene 불검출, chrysene 불검출, benzo(b)fluoranthene $0.0009{\mu}g/kg$, benzo(k)fluoranthene 불검출, benzo(a)pyrene $0.01{\mu}g/kg$, dibenzo(a,h)anthracene 불검출, benzo(g,h,i)perylene 불검출, indeno(1,2,3-c,d) pyrene 불검출이었다. 조리패류에서 개별 PAH 평균 농도는 benzo(a)anthracene $1.84{\mu}g/kg$, chrysene $3.51{\mu}g/kg$, benzo(b)fluoranthene $0.81{\mu}g/kg$, benzo(k)fluoranthene $0.38{\mu}g/kg$, benzo(a)pyrene $0.39{\mu}g/kg$, dibenzo(a,h)anthracene $0.04{\mu}g/kg$, benzo(g,h,i)perylene $0.20{\mu}g/kg$, indeno(1,2,3-c,d)pyrene 불검출이었다.

• 분석과학
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• 제21권6호
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• pp.518-525
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• 2008

포도, 고추, 배추, 토마토 및 감자 등 5종 농산물에 대하여 mandelamide계 신규 살균제인 mandipropamid의 잔류분석법을 확립하였다. 각 농산물을 세절한 시료에 methanol을 가하고 고속마쇄하여 잔류분을 추출하였다. 추출액을 포화식염수와 증류수로 희석하고 dichloromethane으로 분배하여 극성분순물을 제거하였으며, Florisil 흡착크로마토그래피법으로 추가 정제하였다. Mandipropamid의 HPLC/UV 검출기상 최소검출량은 2 ng (S/N>10, 0.01 AUFS)이었고 시료추출물 중 불순물에 의한 간섭은 관찰되지 않았다. 무처리 포도, 토마토, 고추, 배추 및 감자에 대하여 2수준 3반복으로 회수율을 산출한 결과 각각 $99.8{\pm}1.7$ (n=6), $89.3{\pm}5.3$(n=6), $98.7{\pm}2.2$ (n=6), $99.7{\pm}6.8$ (n=6) 및 $91.1{\pm}3.1$ (n=6)이었으며, 분석법의 정량한계는 0.02~0.04 mg/kg이었다. 아울러 검출된 잔류분은 재확인을 위하여 selected-ion monitoring (SIM)을 이용한 LC/MS법을 추가로 확립하였다. 본 연구에서 확립된 mandipropamid의 잔류분석법은 검출감도 및 재현성을 고려할 때 공정분석법으로 사용이 가능하였다.

• 한국축산식품학회지
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• 제29권4호
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• pp.482-486
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• 2009

The aim of this study was to optimize a simple, fast, and economical analysis procedure for the determination of 16 different pesticides in raw milk via GC/MSD. Analyses were performed via gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode (GC/MSD-SIM) using Pentachloronitrobenzene as the internal standard. The modified sample preparation methodology was based on the Pesticide Analytical Manual (PAM) of the FDA concerning fat extraction, ACN-ether partitioning, and clean-up of the Sep-Pak florisil cartridge. The modified methodology for the determination of the 16 pesticides was validated. The range of LOQs of the 16 pesticides was likely three times lower than their Maximum Residence Levels (MRLs). The recoveries of most of the pesticides were acceptable at the fortification levels of 0.5 and 1.0 ${\mu}g/mL$ and their RSD (%) level was less than 20%. None of the 16 pesticides were detected in the selected raw milk samples.

• Journal of Nutrition and Health
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• 제16권2호
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• pp.107-114
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• 1983

There has been no specific test available for identifying the sesame oil among common edible oils. As the contents of sesamin and the ratio of sterols allowed the estimation for the genuine sesame oil, the author investigated to establish some instrumental methods for verification of genuine sesame oil and its distribution in the market. The sesame oil was saponified and the sesamin and sterols were isolated from the unsaponiable fraction by Florisil column chromatography. The individual components were determined by gas- chromatography and sesamin standard (purified sesamin) was obtained by silicagel column chromatography. The gas- chromatographic condition using Flame Ionization Detector supported on 10% OV-101 with di-(2-ethylhexyl) sebacate as an internal standard was suitable, and quantitation of sesamin and sterols, including campesterol, stigmasterol and ${\beta}-sitosterol$ was carried out. The results of this study showed that contents of sesamin in genuine sesame oil were 0.3-0.5% and the ratio of stigmasterol to compesterol was 0.3-0.6 and ${\beta}-sitosterol$ to campesterol 3.0-3.8. The 50 samples from the markets in Seoul were composed of 70% genuine sesame oil, and others were mixed with palm oil, rape seed oil and soybean oil.

• 한국식품위생안전성학회지
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• 제23권1호
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• pp.26-30
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• 2008

다환방향족탄화수소는 환경오염이나 식품의 제조공정 과정 중에 생성될 수 있으며, 홍삼은 수증기로 찌고 건조하여 만들어진다. 시료를 핵산으로 추출한 후 물로 세척하고 후로리실 SPE 카트리지로 정제한 후 고속액체크로마토그래피/형광검출기로 분석하였다. 이동상으로는 아세토니트릴과 물의 혼합용액(8:2)을 사용하였으며 형광검출기의 여기파장은 294 nm이었고 형광파장은 404 nm이었다. 평균 회수율은 105%이었으며, 상대표준편차는 0.5이었다. 대상 식품인 홍삼음료 중 벤조피렌은 검출되지 않았다.

• Journal of Nutrition and Health
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• 제13권4호
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• pp.159-166
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• 1980

Methods for the determination of sterols in sesame oils were studied. The sesame oils were saponified and the sterols isolated from the unsaponifiable matter by Florisil column chromatography, and the individual components were determined by means of gas chromatography. Campesterol, ${\beta}-sitosterol$, stigmasterol were found in sesame oil including unknown Ⅰ and Ⅱ. The use of SE-30 gas chromatographic column allows the slow elution, duplication of peaks and relatively low reproducibility, therefore, 3% OV-17 was suitable for the sterol analysis. The result of this study showed that contents of sterols in sesame oil were campesterol 8.4%, stigmasterol 4.5%, ${\beta}-sitosterol$ 33.9% and others 53.0% involving 8.8% of unknown I and 44.3% of unknown Ⅱ. There has been no specific test available for identifying the sesame oil among common edible oils. But the ratio of sterols in sesame oils allowed the estimation of genuiness. The ratio of sterols vs. campesterol in genuine sesame oils were stigmasterol 0.3- 0.6, ${\beta}-sitosterol$ 3.0-3.8 and unknown Ⅱ 3.0, respectively. The 65 samples were composed of genuine sesame oil 40%, mixed rape seed oil 3%, cotton seed oil 1. 5% others were reused soybean oil or re-extracted oil.

• 농업과학연구
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• 제11권2호
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• pp.190-193
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• 1984

쇠비름즙액(汁液)(원액(原液))은 사과 부란병균(病菌)(Valsa mali), 배 검은무늬병균(病菌)(Alternaria kikuchiana), 벼 도열병균(病菌)(Pyricularia oryzae)등 몇가지 식물병원균(植物病原菌)에 대한 항균작용(抗菌作用)을 지니고 있다. 이와 같은 항균작용(抗菌作用)을 나타내는 물질(物質)은 메타놀에 잘 용해(溶解)되며 지질(脂質)에 속하는 물질(物質)로 추정(推定)된다. 그리고 쇠비름즙액(汁液)에 함유(含有)되어 있는 항균물질(抗菌物質)은 균채신장억제(菌采伸長抑制) 뿐만 아니라 포자발아억제(胞子發芽抑制) 효과(效果)를 보여주고 있다.

• 한국환경농학회지
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• 제29권3호
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• pp.247-256
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• 2010

A high-performance liquid chromatographic (HPLC) method was developed to determine buprofezin residues in hulled rice and fruits. The buprofezin residue was extracted with acetone and the extract was stepwise purified by liquid-liquid partition and Florisil column chromatography. For rice samples, acetonitrile/n-hexane partition was additionally employed to remove nonpolar lipids. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate buprofezin from sample co-extractives, as detected by ultraviolet absorption at 250 nm. Recovery experiment at the limit of quantitation validated that the proposed method could evidently determine the buprofezin residue at the level of 0.02 mg/kg. Mean recoveries from hulled rice, apple, pear, and persimmon samples fortified at three tenfold levels were in the range of 80.8~85.2%, 89.1~98.4%, 88.8~95.7% and 90.8~96.2%, respectively. Relative standard deviations of the analytical method were all less than 5%, irrespective of sample types. A selected-ion monitoring LC/mass spectrometry with positive electrospray ionization was also provided to sensitively confirm the suspected residue.

• 생약학회지
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• 제32권3호통권126호
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• pp.200-211
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• 2001

This study was carried out to determine the 11 organochlorine, 7 organophosphorus residual pesticides in 251 crude drugs. These residual pesticides in herbal drugs were extracted with acetonitrile and the extracts were cleaned up via LC-florisil solid phase extraction column. The prepared samples were assayed for pesticide residues using GC-ECD, NPD with capillary column and identified by GC-MSD. Recoveries were $63.9{\sim}111.5%$ in the organochlorine pesticides and $69.8{\sim}92.4%$ in the organophosphorus pesticides, and detection limits were $0.001{\sim}0.65\;ppm$ in the organochlorine pesticides and $0.0009{\sim}0.0074\;ppm$ in the organophosphorus pesticides. Pesticide residues were detected in 9 cases.