• Analytical Science and Technology
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• v.26 no.2
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• pp.142-153
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• 2013

A new, rapid, and simple analytical method was developed and validated using high performance liquid chromatograph-photodiode array detector (HPLC-PAD) for the determination of lepimectin residues in agricultural commodities. The lepimectin residues in samples were extracted with methanol, partitioned with dichloromethane, and then purified with glass column filled with subsequently to aminopropyl ($NH_2$) solid phase extraction (SPE) cartridge. The purified samples were detected using HPLC-PAD. Correlation coefficient ($R^2$) of both lepimectin $A_3$ and $A_4$ solutions were 0.9999. The method was validated using cucumber spiked with lepimectin at 0.02 and 0.2 mg/kg and pepper, mandarin, hulled rice, potato, soybean at 0.02 and 0.5 mg/kg. Average recoveries were 76.0~114.8% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.01 mg/kg, respectively. The result of recoveries and overall coefficient of variation of a laboratory results in Gwangju regional KFDA and Daejeon regional KFDA was followed with Codex guideline (CAC/GL 40). Therefore, developed method in this study is accurate, rapid, and appropriate for lepimectin determination and will be used to keep safety of lepimectin residues in agricultural products.

• The Microorganisms and Industry
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• v.35 no.1
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• pp.4-9
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• 2009

• Korean Journal of Veterinary Research
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• v.39 no.3
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• pp.609-615
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• 1999

From July of 1997 to June of 1998, total 279 raw milk samples over withdrawal period after mastitis treatment from dairy farms located in the provinces of Kyonggi and Choongchung were collected to test drug residues. Each sample was tested by TTC- II test and Delvotest SP. Among the total 152 raw milk samples of cow treated by ${\beta}$-lactams, 32 samples(21.2%) were positive on the Delvotest and 15 samples(9.9%) showed positive on the TTC-II test. Also, from the total 37 samples treated by sulfonamides, 5 samples(13.5%) were positive on the Delvotest and 3 samples(8.1%) showed positive on the TTC-II test. For the total 55 raw milk samples of cow treated by tetracyclines, 9 samples(16.4%) were positive on the Delvotest and 5 samples(9.1%) showed positive on the TTC-II test. In addition, from the total 35 samples treated by aminoglycosides, 7 samples(20.0%) were positive on the Delvotest and 5 samples(14.3%) showed positive on the TTC-II test. Our study shows that it is possible that drugs are to be detected by the drug residues test of an individual raw milk even over the withdrawal period after mastitis treatment and the raw milk of bulk tank.

• Journal of Food Hygiene and Safety
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• v.28 no.3
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• pp.222-226
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• 2013

A simple and sensitive analytical method was developed using gas chromatograph with electron capture detector (GC-ECD) and gas chromatograph-mass spectrometer (GC-MS) for determination and identification of chloropicrin. Because of small molecular weight and high volatile properties of chloropicrin, analytical method was developed utilizing headspace extraction and direct injection to the GC. The developed method was validated using hulled rice sample spiked with chloropicrin at different concentration levels, 0.1 and 0.5 mg/kg. Average recoveries of chloropicrin (using each concentration three replicates) ranged 77.7~79.3% with relative standard deviations less than 10% and calibration solutions concentration in the range $0.005{\sim}0.5{\mu}g/mL$, and limit of detection (LOD) and limit of quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The result showed that developed analytical methods was successfully applied to detect a small amount of chloropicrin in hulled rice.

• Korean Journal of Food Science and Technology
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• v.46 no.1
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• pp.7-12
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• 2014

A sensitive and simple analytical method to identify flutianil residues in agricultural commodities was developed and validated using gas chromatography-electron capture detection (GC-ECD) and mass spectrometry (GC-MS). The flutianil residues were extracted with acetonitrile, partitioned with dichloromethane, and then purified using a silica solid-phase extraction (SPE) cartridge. The method was validated using pepper, sweet pepper, mandarin, hulled rice, soybean, and potato spiked with 0.02 or 0.2 mg/kg flutianil. The average recovery of flutianil was 76.5-108.0% with a relative standard deviation of less than 10%. The limit of detection and limit of quantification were 0.004 and 0.02 mg/kg, respectively. The result of recoveries and relative standard deviation were in line with Codex Alimentarius Commission Guidelines (CAC/GL 40). These results show that the method developed in this study is appropriate for flutianil identification and can be used to maintain the safety of agricultural products containing flutianil residues.

• Journal of Food Hygiene and Safety
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• v.28 no.3
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• pp.213-216
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• 2013

Antibiotic Detection Kit (Combination I), a lateral flow immunoassay (LFIA) developed for the detection of antibiotic residues in milk, was utilized for the analysis of antibiotic residues in the muscle tissue of olive flounder. After 60-min treatment by dipping in water dosed with ampicillin (200-g/ton water), the residue depletion of ampicillin was investigated in 25 cultured olive flounder (Paralichthys olivaceus). Muscles of fish were sampled on the 1st, 2nd, 3rd, 4th and 5th day after drug treatment. The concentration of ampicillin in the muscle was determined by LFIA. The absorbance ratio of the sample to the control blank (Bs/Bo) was employed as an index to determine the muscle residues in olive flounder. To investigate the recovery rate, standard solutions were added to muscle samples to give final concentrations in the muscle of 4 and 8 ng/ml. The recovery rates of all spiked samples were > 96% of the spiked value. Ampicillin was detected in the muscle of fish treated with the drug until the 2nd day of the withdrawal period. The present study showed that the LFIA can be easily adopted to predict ampicillin residues in tissue of farmed fishes.

• Asian-Australasian Journal of Animal Sciences
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• v.13 no.12
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• pp.1775-1778
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• 2000

Oxytetracycline has been widely used in the cattle industry to control pneumonia, shipping fever, foot rot, bacterial enteritis, and uterine infections. Extensive use of antibiotics in veterinary clinics has resulted in residues in tissue and bacterial resistance to antibiotics. To prevent unwanted drug residues from entering the human food chain, extensive control measures have been established by both government authorities and industries. The demands for reliable, simple, sensitive, rapid and low-cost methods for residue analysis of foods are increasing. In this study, we established a rapid test for tissue residues of oxytetracycline in cattle. The recommended therapeutic dose of oxytetracycline (withdrawal time, 14 days) was administered to 10 cattle. Blood samples were collected from each cow before drug administration and during the withdrawal period. The concentration of oxytetracycline in plasma, determined by a semi-quantitative ELISA, was compared to that of the internal standard, 10 ppb. The absorbance ratio of internal standard to sample (B/Bs) was employed as an index to determine whether the residues in cattle tissues were negative or positive. That is, a B/Bs ratio less than 1 was considered as residue positive and that greater than 1 as negative. Based on this criterion, all plasma samples from cattle were negative to oxytetracycline at pre-treatment. Oxytetracycline could be detected in the plasma treated cattle until day 14 post-treatment. The present study showed that the semi-quantitative ELISA could be easily adapted in predicting tissue residues for oxytetracycline in live cattle.

• Korean Journal of Pharmacognosy
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• v.31 no.4
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• pp.455-458
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• 2000

Research on pesticide residues as endocrine disruptors in natural medicines was initiated by Korea Food & Drug Administration this year. We determined the presence and levels of certain pesticides in selected natural medicines. The natural medicines collected this year are Glycyrrhiza Root, Cinnamon Bark, Pueraria Root, Polygonatum Rhizome, Jujube, Schizandra Fruit, Lycium Fruit, Liriope Tuber, Eucommia Bark, Peony Root, Korean Angelica, Dioscorea Rhizome, Cnidium Rhizome, Cassia Seed, Platycodon Root, Comus Fruit, Mentha Herb, Epimedium Herb, Bupleurum Root, and Ginger, which have no data for pesticide residues and 192 samples of them were circulated in Korea, 28 samples were circulated in China. In order to analyze many pesticides in large number of samples we used simultaneous multi-residue analysis of pesticides by GC-ECD, which was followed by GC-MSD analysis to confirm the identity of the detected pesticide in each sample.

• Korean Journal of Veterinary Research
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• v.48 no.2
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• pp.175-179
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• 2008

Parallux, a solid-phase fluorescence immunoassay (SPFIA) developed for detection antibiotics residue in milk, was applied for analysis of antibiotics in muscle tissue of olive flounder (Paralichthys olivaceus), rockfish (Sebastes schlegeli), and red sea bream (Pagrus major). Fishes were dipped in neomycin 140 mg/ton water, the recommended therapeutic dose, for 24 h. Muscle samples were obtained on 1st, 2nd, 3rd, 4th and 5th day after drug treatment. The concentration of neomycin in muscle was determined using an internal standard (100 ppb as neomycin). The absorbance ratio of sample to internal standard (S/C) was employed as an index to determine the muscle residues in fishes. To investigate the recovery rate, the standard solutions were added to muscle samples to give final concentrations in muscle of 0.2 and 0.5 mg/ml. The recovery rates of all spiked samples were > 85% of the spiked value. Neomycin was detected in muscles of fishes treated after the 1st day of withdrawal period. On the 2nd day after drug treatment, all muscle samples showed negative reaction (S/C ration ${\leq}$ 1.0). The present study showed that the SPFIA can be applied for predicting residues of neomycin in muscle tissues of farmed fishes.

• Korean Journal of Environmental Agriculture
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• v.30 no.4
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• pp.432-439
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• 2011

BACKGROUND: An official analytical method was developed to determine etofenprox residues in agricultural commodities using high-performance liquid chromatography (HPLC). METHODS AND RESULTS: The etofenprox residue was extracted with acetone from representative samples of five raw products which comprised rice grain, apple, mandarin, cabbage, and soybean. The extract was then serially purified by liquid-liquid partition and Florisil column chromatography. For rice and soybean samples, acetonitrile/n-hexane partition was additionally coupled to remove nonpolar lipids. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate etofenprox from co-extractives. Intact etofenprox was sensitively detected by ultraviolet absorption at 225 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine the etofenprox residue at 0.02 mg/kg. Mean recoveries from five crop samples fortified at three levels in triplicate were in the range of 93.6~106.4%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types. A selected-ion monitoring LC/mass spectrometry with positive atmospheric-pressure chemical ionization was also provided to confirm the suspected residue. CONCLUSION(s): The proposed method is simple, rapid and sensitive enough to be employed in routine inspection or monitoring of agricultural products for the etofenprox residue.