• 한국환경과학회지
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• 제12권4호
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• pp.477-480
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• 2003

Pesticides were extracted from samples with 70% acetone and methylene chloride in order, and then cleaned up via open-column chromatography apparatus packed with florisil, and finally analyzed simultaneously the organochlorine and pyrethroid pesticides using GC(ECD). An ultra-2 fused silica capillary column was used to separate and identify the products. The resolution between the last isomeric peak of cypermethrin(59.987min) and the first isomeric peak of flucythrinate(60.043min) was not satisfactory. The last isomeric peak of fenvalerate(62.344min) and the first isomeric peak of fluvalinate(62.397min) were overlapped. Recoveries of soybean sample fer the most pesticides were 73.3% to 102.4%. Detection limits were between 0.004 and 0.063 ${\mu}$g/mg when this method was used.

• 한국환경보건학회지
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• 제23권1호
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• pp.66-73
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• 1997

This procedure describes the method for gas chromatographic determination of 31 organophosphorus and 28 organochlorine pesticides in 10g of spinach, tomato and onion. After the pesticides were extracted with several solvents, the amount of coextractives and recovery rates of acephate and methamidophos were calculated. Samples for organochlorine pesticides were cleaned up with florisil solid phase extraction columns. NaBH$_4$ was added to onion extracts, which contained sulfur compound. All the concentrated extracts were analyzed by gas chromatography with ECD and NPD. The smallest amount of coextractives resulted from the spinach samples extracted with 5% MeOH in ethyl acetate. 5% EOH in ethyl acetate had the highest extractability for acephate and methamidophos and gave the best overall performance as an extraction solvent. The ability of 5% EOH in ethyl acetate to extract various organophosphorus and organochlorine pesticides from spinach, tomato and onion was examined. Recovery of 59 insecticides ranged from 58.0% to 110.5%. The average recoveries of fortified spinach, tomato and onion were 90.08%, 94.54% and 84.90%, respectively.

• Journal of Applied Biological Chemistry
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• 제43권2호
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• pp.94-100
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• 2000

An analytical method was developed to determine abamectin and milbemectin residues in apple, pear, and citrus using HPLC with ultraviolet absorption detection. Abamectin and milbemectin were extracted with methanol from apple, pear, and citrus samples. The extract was diluted with saline water and dichloromethane partition was followed to recover the compounds from the aqueous phase. Florisil column chromatography and aminopropyl solid-phase extraction were employed as cleanup methods to remove most of co-extractives from the sample extract. Reverse-phase HPLC using an octadecylsilyl column was successfully applied to separate and quantitate abamectin and milbemectin residues in sample extracts at the wavelength of 245 nm. Recoveries of abamectin and milbemectin from fortified samples ranged 80.4~90.3% and 90.9~96.8%, respectively. Relative standard deviations of the analytical method were less than 10% for both acaricides. Detection limit of the analytical method was 0.003 mg/kg sample for all the analytes. The proposed method was reproducible and sensitive enough to evaluate terminal residues of abamectin and milbemectin in apple, pear, and citrus.

• Journal of Applied Biological Chemistry
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• 제42권4호
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• pp.191-196
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• 1999

A multiresidue analytical method was developed for eight acaricides including benzoximate, clofentezine, fenazaquin, fenothiocarb, fenpyroximate, hexythiazox, pyridaben, and tebufenpyrad in four major fruits using high-performance liquid chromatography (HPLC). All the confounds were extracted with acetone from apple, pear, grape, and citrus samples. The extract was diluted with saline water, and n-heaxane partition was followed to recover the acaricides. Florisil column chromatography was employed to further purify the sample extract. HPLC with ultraviolet absorption detection, using an octadecylsilyl column under the isocratic mobile phase of acetonitrile/water mixture, was successfully applied to separate and quantitate all the compounds in the purified extract. Recoveries of the eight acaricides from for fortified samples ranged 86.4~97.0%. Relative standard deviations of the analytical method were all less than 10%. Detection limits of the method were in the range of 0.02~0.05 mg/kg. The proposed method was reproducible and sensitive enough to evaluate the terminal residue of the eight acaricides in the fruit harvest.

• 한국환경과학회지
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• 제12권10호
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• pp.1117-1120
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• 2003

Pesticides were extracted from samples with 70% acetone and methylene chloride in order, and then cleaned up via open-column chromatography apparatus packed with florisil, and finally analyzed simultaneously the organophosphorus pesticides using GC/NPD. Ultra-2 and Ultra-1 fused silica capillary columns were used to separate and identify the products. Recovery of most analytes from soybean sample, taken from pesticide residues well, was greater than(80%) for all except(6) analytes. This method can simultaneously determine multiple pesticides with a high degree of accuracy and precision.

• Preventive Nutrition and Food Science
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• 제4권4호
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• pp.270-275
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• 1999

Radiation-induced hydrocarbons and 2-alkylcyclobutanones are formed from the fatty acids of irradiated fats. Peanuts were irradiated with a dose of 0.1∼10 kGy. The method consists of the extraction of fat from peanuts, separation of hydrocarbons and 2-alkylcyclobutanones with florisil column chromatography and identification of hydrocarbons by the GC/MS method and 2-alkylcyclobutanones by GC/MS/selected ion monitoring (SIM). Concentrations of hydrocarbons and 2-alkylcyclobutanones were linearly increased with the dose levels of radiation. The major hydrocarbons in the irradiated peanut samples were 8-heptadecene and 1,7-hexadecadiene from oleic acid and 6,9-heptadecadiene and 1,7,10-hexadecatriene from linoleic acid. 2-(5'-Tetradecenyl)cyclobutanone, one of 2-alkylcyclobutanones, was the highest amount in the irradiated peanuts. Radiation-induced hydrocarbons in the peanuts were detected at doses of 0.5 kGy and over, and radation-induced 2-alkylcyclobutanones were detected at doses of 1 kGy and over. These compounds were not confirmed in unirradiate peanuts.

• 한국식품영양과학회지
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• 제26권6호
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• pp.1109-1115
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• 1997

Hydrocarbons were analyzed in irradiated beef, pork, dried and seasoned beef, dried anchovy, dried squid, dried shrimp, and fish paste to determine whether the hydrocarbons can be used as markers for detecting post-irradiation of the imported meat and fish products. The samples were irradiated at 0.5, 1, 3, and 6 kGy. Fat was extracted with hexane, and hydrocarbons were separated from the fat through Florisil column. The hydrocarbons were analyzed with GC. Hydrocarbons 15:0, 16:1, 17:1, 16:2, 17:2, and 16:3 in beef and pork, 17:1, 16:2, and 17:2 in dried and seasoned beef, 16:2 in dried anchovy, 16:1 and 17:1 in dried squid, 16:1, 17:1, and 16:2 in dried shrimp, and 16:1, 16:2, and 16:3 in fish paste were detected in the irradiated samples, but not in the unirradiated, so that the hydrocarbons may be used as makers for detecting post-irradiation of each item.

• 농약과학회지
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• 제19권3호
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• pp.195-203
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• 2015

본 연구에서는 GC-ECD/MS를 이용하여 농산물 중 aromatic 살균제 quintozene의 잔류 분석법을 확립하였다. 대표 농산물은 사과, 고추, 배추, 현미 및 콩을 선정하였고, acetonitrile을 가하여 추출된 quintozene 성분을 n-hexane 액-액 분배법과 florisil 흡착크로마토그래피법으로 정제하여 GC-ECD/MS 분석대상 시료로 사용하였다. Quintozene의 정량적 분석을 위한 최적 GC-ECD 분석 조건을 확립하였으며, 정량한계(LOQ)는 0.004 mg/kg 이었다. 각 대표 농산물에 대해 정량한계, 정량한계의 10배 및 50배 수준에서 회수율을 검토한 결과 모든 처리농도에서 79.9~102.7% 수준을 나타내었으며, 반복 간 변이계수(CV)는 최대 4.3%를 나타내어 잔류분석 기준인 회수율 70~120% 및 분석오차 10% 이내를 충족시키는 만족한 결과를 도출하였으며, GC/MS/SIM을 이용하여 실제 농산물 시료에 적용하여 재확인 하였다. 이상의 결과로 신규 quintozene의 GC-ECD/MS 분석법은 검출한계, 회수율 및 분석오차면에서 국제적 분석기준을 만족하는 신뢰성이 확보된 정량 분석법으로 사용 가능할 것이다.

• 한국식품저장유통학회지
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• 제21권6호
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• pp.859-865
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• 2014

본 연구는 호두를 대상으로 감마선을 1-10 kGy 선량으로 조사시켜 생성된 hydrocarbon류와 2-alkylcyclobutanone류를 통해 방사선 조사여부를 확인하였다. 지방은 soxhlet방법으로 n-hexane을 추출용매로 사용하였고 florisil이 충진된 column으로 분리하여 gas chromatography / mass spectrometry(GC/MS)로 확인하였다. 감마선 조사된 호두에서 검출된 주요 hydrocarbon류는 oleic acid에서 유도된 8-heptadecene과 linoleic acid에서 유도된 8,11-Heptadecadiene, 1,7,10-Hexadecatriene이었고, 검출된 주요 2-alkylcyclobutanone류는 linoleic acid와 oleic acid에서 유도된 2-(5',8'-tetradecadienyl)cyclobutanone(5',8'-TCB), 2-(5'-tetradecenyl) cyclobutanone(TECB)가 가장 높은 함량으로 확인되었다. 조사된 호두에서 생성된hydrocarbon류와 2-alkylcyclobutanone류의 생성량은 선량에 비례하여 증가하였으며, 이 화합물들은 1 kGy 이상 조사된 시료에서만 나타났으며 비조사 시료에서는 확인되지 않았다. 따라서 방사선 조사에 의해 oleic acid과 linoleic acid에서 유도된 hydrocarbon류 중 8-heptadecene, 8,11-Heptadecadiene 및 1,7,10-Hexadecatriene, 2-alkylcyclobutanone류 중 5',8'-TCB 및 TECB는 감마선 조사 여부의 확인을 위한 marker로서 활용가능성이 높게 나타났다.

• 분석과학
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• 제25권6호
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• pp.364-369
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• 2012

Isotianil은 쌀 도열병을 방제하기 위한 새로이 개발된 식물활성 살균제로 다른 식물활성제에 비해 소량으로도 장시간의 효과를 나타내는 특징을 가지고 있다. 신규 농약 Isotianil에 대한 기준은 국내의 경우 2010년 쌀에 대하여 0.1 mg/kg으로 최초 설정되었으며, 이에 따른 식품 중 안전관리를 위해 Isotianil을 분석하기위한 검사법을 개발하였다. 검체 일정량에 acetonitrile을 가하고 균질화하여 대상농약을 추출하였으며, 액-액분배하고 florisil 카트리지를 이용한 고체상 추출 후 GC-NPD 및 GC-MSD로 분석하였다. 분석결과 농산물에 의한 간섭물질은 없었으며, 대표 농산물 현미 등 6 종에 대한 Isotianil의 분석 시험법의 정량한계와 직선성은 각각 0.05 mg/kg과 0.999($r^2$)이었다. 회수율은 대표 농산물에서 70.0~103.9%이었으며, 분석오차는 10% 미만으로 CODEX 잔류분석 기준에 적합하였다.