• The Korean Journal of Pesticide Science
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• v.19 no.4
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• pp.345-353
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• 2015

The aim of this study is to develop residue analysis method for fenoxanil, a MBI (melanin biosynthesis inhibitor) propionamide fungicide, had mainly been used to control rice blast, and disease of other crops, fruits, and vegetables by using GLC/NPD and GC/MS. Extraction with acetone and partition with n-hexane/dichloromethane (80/20, v/v) were performed from hulled rice, soybean, Kimchi cabbage, green pepper, and apple, then column clean-up with florisil was applied. Mean recoveries were 82.2%-109.1% with less than 7.2% of coefficients of variation and limit of quantitation was set at the concentration of 0.04 mg/kg from the five agricultural products through the determination by GLC/NPD equipped with DB-5 capillary column and single laboratory validation. As a confirmatory method, GC/MS selected ion monitoring (SIM) was set from m/z 125.0, 188.9, and 293.0. Developed method is expected to apply the single residue analysis of fenoxanil in agricultural products.

• Applied Biological Chemistry
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• v.20 no.2
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• pp.236-241
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• 1977

Analytical method of carbofuran (2,3-dihydro-2, 2-dimethyl-7-benzofuranyl methyl carbamate) residues and its persistence in rice seeds, rice seedlings, rice plants and soils were studied by gas-liquid chromatographic analysis using electron capture detector. 1. The effective column material for clean-up is Florisil (5% $H_2O$)+Alumina (4% $H_2O$)+absorbent mixture with rinsing the first 300l of eluants to remove impurities in the column materials. 2. The method of applying an gelatin encapsulated carbofuran to the root zone of rice plant is the longest persistence in its residues. 3. By seed treatment, no carbofuran residues were detected in rice seeds and seedlings. 4. The amounts of carbofuran residues in rice seedlings is in proportion to the soaking time of rice seedlings in carbofuran solution rather than the concentration of the chemical. 5. Applying carbofuran by root zone has the higher and the loger residual effect than broadcast. 6. Persistence of carbofuran in the high clay content soil is longer than in the low clay content soil. 7. No carbofuran residue was detected in rough rice at havesting time.

• Korean Journal of Food Science and Technology
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• v.40 no.3
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• pp.354-359
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• 2008

A survey for zearalenone contamination was conducted on 27 soy bean samples, 27 red bean samples, 16 black bean samples, 19 seoritae samples, 14 seomoktae samples, for a total of 127 commercial Korean samples. Zearalenone was quantified by the immunoaffinity column clean-up method with high performance liquid chromatography-fluorescence detection (HPLC-FLD), and was confirmed by liquid chromatography tandem mass spectrometry(LC-MS/MS). The limits of detection and quantification were $2.0{\mu}g/kg$ and $6.0{\mu}g/kg$, respectively. The recovery in the beans ranged from 82.2 to 98.4%. According to HPLC-FLD, zearalenone was detected in 13 samples (10.2% incidence), including 1 soybean and 12 red bean samples. The zearalenone contamination levels were in the range of 8.01${\sim}38.98{\mu}g/kg$. Finally, LC-MS/MS analysis was conducted in the contaminated samples to verify the results of HPLC-FLD. The LC-MS/MS results confirmed the presence of zearalenone in all 13 samples. The contamination level was lower than that of EU, which is below $100{\mu}g/kg$ for raw grains.

• Journal of Food Hygiene and Safety
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• v.24 no.2
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• pp.169-173
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• 2009

A survey of total aflatoxin levels was conducted on 145 samples(carthamiflos, thujae semen, giycyrrhizae radix et rhizoma) collected in Yakyeang markets in Seoul. Aflatoxin levels were quantified by the immunoaffinity column clean-up method followed by performance liguid chromatography(HPLC)-fluorescence detector(FLD). Aflatoxins were found in 10(6.9%)samples including 5 Arecae semen, 4 Thujae semen, 1 Zizyphi semen with a range of $0.45{\sim}79.15\;{\mu}g/kg$. Generally These results show that the contamination level of aflatoxins in Herb Medicines consumed in Korea is high compared with the standard in Korea Herb Medicine Code($10\;{\mu}g/kg$ as aflatoxin B1). It is considered that aflatoxin concentration was increased in herb medicines during a storage and drying in herb medicines examined

• The Korean Journal of Pesticide Science
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• v.19 no.4
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• pp.370-393
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• 2015

This study was conducted to compare STQ method, multi-residue method in Korean food code and QuEChERS method for validated selected and accuracy, reproducibility and efficiency. A total of 45 selected and targeted pesticides were the analyzed by GC and 5 of them were crops (apple, potato, green pepper, rice, soy bean). $R^2$ values were calculated in the standard calibration curve was over 0.990. Recovery tests were performed by three replications in two levels and the relative standard deviation of the repeated experiments was less than 30%. The average percentage of recoveries in the multi-residue method in Korean food code was 89.13%, QuEChERS method was 92.45% and STQ method was 85.28%. In addition, matrix effects in multi-residue method in Korean food code was 24.61%, QuEChERS method was 23.98% and STQ method showed 11.24%. The STQ method is easy and showed high clean-up effect in extracting the sample solution than the QuEChERS method and clean-up with C18, PLS, PSA cartridge columns. A large volume of the sample was injected in order to compensable for the problem, that occurred due to high detection limit in the analyser. When the STQ method was applied using a large volume injector, the standard calibration curve showed a higher linearity $R^2=0.990$, and method detection limit was 0.01 mg/kg. It showed an average recovery of 91.84% and the relative standard deviations of three replications repeated in two level process was less than 30% and had an average matrix effect of 17.90%.

• Korean Journal of Veterinary Service
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• v.39 no.3
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• pp.167-174
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• 2016

In this study, we analyzed for the changes of low organic compounds during 4 weeks incubation though inoculation of harmful microorganisms on commercial feed. Two percent of overnight cultures of Exiguobacterium acetylicum, Acinetobacter calcoaceticus, Aspergillus flavus and Fusarium graminearum were inoculated in feed, respectively. After adjusting moisture level to 50% for the promotion of feed spoilage, pH was decreased to 4.58~5.03 and microorganism was ranged to $6{\sim}10log_{10}CFU/g$. The compounds were compare between aflatoxin G1 producing feeds and aflatoxin G1 non-producing feeds. Aflatoxins G1 were detected by the immunoaffinity column clean-up method with HPLC-FLD, and were confirmed in samples incoulated by Aspergillus flavus and Acinetobacter calcoaceticus. Koiganal II, cyclohexanol and butadien-one were detected from samples (the non-sterilized inoculated feed) by Aspergillus flavus and Acinetobacter calcoaceticus. Respectively as aflatoxin G1 pre-detected substance, Koiganal II, cyclohexanol and butadien-one may be useful substance for the pre-detection of aflatoxin G1.

• Analytical Science and Technology
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• v.15 no.3
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• pp.300-316
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• 2002

The extraction methods of PBBs from environmental samples by soxhlet extraction for solid phase and liquid-liquid extraction for liquid phase were compared. After extraction, silicagel and florisil as column clean up methods were used for the comparison of cleanup efficiency with different solvent system. Also, the analytical instruments were used GC/MSD. The 22 kinds of PBBs standards were used to establish the analytical methods to perform the experiments of recoveries and detection limits in water and soil. The detection limits of PBBs represented 5~10 ng/L for water and 0.5~3.5 ng/g for soil samples, respectively. The recoveries of water samples represented 96~107% in n-hexane, dichloromethane and toluene for water, and 60~80% in combined solvent with n-hexane and acetone. The recoveries of soil sample were surveyed 67~97% in soxhlet extraction and 64~76% in ultrasonic extraction with selected solvents.

• Analytical Science and Technology
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• v.13 no.5
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• pp.666-674
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• 2000

The present study describes an analytical method for the determination of polybrominated biphenyls (PBBs) in biota samples by gas chromatography-mass spectrometry (GC/MS). PBBs are extracted twice from 20 g samples with mixture solvent 40mL acetone and 80mL hexane using ultrasonic agitation for 20 min. Lipids in extracts are degraded by concentrated sulfuric acid and then PBBs are purified with Florisil column. The purified extracts are analyzed by GC/MS-selected ion monitoring mode for the quantitation of PBBs in biota sample. The overall recovery yields of PBBs range between 77 and 111% under these experimental conditions.

• Korean Journal of Veterinary Research
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• v.60 no.4
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• pp.209-213
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• 2020

This study examined the residue of dl-methylephedrine hydrochloride (MEP) on the muscle of pigs administered orally with MEP 12 g/ton feed for seven consecutive days. Twenty healthy cross swine were administered MEP. Four treated animals were selected arbitrarily to be sacrificed at 1, 2, 3, 4, and 5 days after treatment. MEP residue concentrations in the muscle were determined by liquid chromatography coupled with tandem mass spectrometry. The drug was extracted from muscle samples using 10 mM ammonium formate in acetonitrile followed by clean-up with n-hexane. The analyte was separated on an XBridgeTM hydrophilic interaction liquid chromatography column using 10 mM ammonium formate in deionized distilled water and acetonitrile. The correlation coefficient (R2) of the calibration curve was 0.9974, and the limits of detection and quantification were 0.05 and 0.15 ㎍/kg, respectively. The recoveries at three spiking levels were 94.5-101.2%, and the relative Standard Deviations was less than 4.06%. In the MEP-treated group, MEP residues on one day post-treatment were below the maximum residue limit in the muscle. The developed method is sensitive and reliable for the detection of MEP in porcine muscle tissues. Furthermore, it exhibits low quantification limits for animal-derived food products destined for human consumption.

• Analytical Science and Technology
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• v.21 no.3
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• pp.174-182
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• 2008

The study on the development of rapid analytical method of PCBs containing waste was performed by considering the extraction, column cleanup process, analytical condition and so on. In the established method, new sample clean-up procedure, new quantification peaks and temperature program were introduced. Method detection limit of the method was 0.5 mg/L, and the method could save the total run time to 2/3, therefore save the analysis cost, The new rapid analytical method of transformer oil was suggested to the waste official test method.