• Korean Journal of Veterinary Research
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• v.36 no.3
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• pp.541-550
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• 1996

Tetracycline antibiotics have been widely used not only therapeutics but feed additives. There are many methods for the isolation and determination of tetracycline antibiotics in animal muscle tissue. But those methods take much time and labor, so it is difficult to analyse many samples simultaneously. A rapid isolation method and liquid chromatographic determination of tetracycline antibiotics in animal muscle tissue (bovine, porcine, chicken) is presented. Blank control and tetracyclines fortified samples (0.5g) were blended with $C_{18}$ containing 0.05g each of oxalic acid and disodium ethylenediaminetetraacetate. After homogenize, homogenate was transferred to glass column made from 10ml glass syringe and compressed to 4~4.5ml volume. A column made from the $C_{18}$/meat matrix was washed with hexane (8ml) and dichloromethane (8ml, if needed), following which the tetracyclines were eluted,vith methanol or 0.01M methanolic oxalic acid (8ml). The eluates containing tetracyclines analytes were free from interfering compounds when analysed by HPLC with UV detection (photodiode array at 360nm). Standard curve for each tetracycline showed a linear response at the range of $0.05{\sim}1.0{\mu}g/ml$ and tetracycline antibiotics were eluted within 4ml of eluted volume. All tetracycline antibiotics except tetracycline were stable during the concentration process at $40^{\circ}C$ and time required for concentration was 3~4 hours. Fortified samples containing oxalic aicd and EDTA represented more good recoveries than those of not-contained sample. Recoveries were 91.8~110.1% (oxytetracycline; OTC), 57.7~79.5% (tetracycline; TC), 78.1~88.6% (chlortetracyclines; CTC) and 88.4~100.6% (doxycycline; DC) in pork tissue, 101.1~126.8% (OTC), 66.4~75.4% (TC), 79.2~88.1% (CTC) and 69.3~86.7% (DC) in beef tissue, and 90.8~95.6% (OTC), 66.2~84.4% (TC), 75.7~77.2% (CTC) and 55.6~80.7% (DC) in chicken muscle tissue. The detection limits validated in muscle tissue by this method were $0.05{\mu}g/g$ for OTC and TC, and $0.1{\mu}g/g$ for CTC and DC.

• Journal of Life Science
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• v.20 no.1
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• pp.60-65
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• 2010

Since organic sulfur compounds respond to GC/ECD sensitively, they interfere with quantitative separation of pesticides during residual pesticide analysis of Allium species. In this study, it was intended to develop a rapid and simple method for pesticide multi-residues analysis through clean-up and interferences by a solid-phase extraction (SPE). An SPE method employing silver nitrate impregnated Florosil cartridge was developed and evaluated for the elimination of sulfur compounds from the test solution of Allium species during pesticide residues analysis. The silver nitrate impregnated Florosil cartridge was prepared by efflux of 3 ml of 20% silver nitrate solution through Florosil cartridge (1 g packing, 6 ml tube). The extracts equivalent to 2, 4 6, and 10 g of each sample were loaded onto the cartridge and allowed to exude, and then the exudations were analyzed by GC/ECD. More than 95% of sulfur compounds were removed from the loaded extracts equivalent, up to 6 g in onion, 4 g in spring onion and 4 g in shallot, respectively. 40 pesticides were spiked in the Allium species and loaded onto the cartridge to determine the recoveries; from this, the recoveries of 34 pesticides were within 70~120%.

• The Korean Journal of Pesticide Science
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• v.16 no.1
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• pp.43-53
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• 2012

In order to monitor the levels of pesticides in environment-friendly stalk and stem vegetables and leafy vegetables selling at markets in Korea. A total of 637 (395 organic agricultural products, 242 pesticide-free agricultural products) samples of 21 stalk and stem vegetables and leafy vegetables were collected twice from markets in July and August 2010 in Korea. Pesticide residues in samples were analyzed by multiresidue method for 240 pesticides using GC-ECD/NPD and HPLC-DAD/FLD. The suspected-pesticides were confirmed with a GC-MSD. As a result of analysis, six pesticides were detected from eight samples, representing a detection rate of 1.3% and amounts of pesticide residues in samples were as follows: alachlor 0.043, chlorfenapyr 0.022-0.324, diazinon 0.024, dicofol 0.009-0.138, dithiopyr 0.008, metolachlor 0.025 mg/kg. Their residue levels were below the MRLs. Estimated daily intakes (EDIs) of the pesticides detected from stalk and stem vegetables and leafy vegetables were less than 25% of their acceptable daily intakes (ADIs), representing that residue levels of the pesticides detected were evaluated as safe for consumption. However, five samples containing pesticide residues were unsuitable environment-friendly products because of pesticides detected more than their 10% MRLs in organic and pesticide-free agricultural products.

• Korean Journal of Environmental Agriculture
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• v.9 no.1
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• pp.15-22
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• 1990

The efects of application time on the persistence of chlorothalonil in sesame plants and its persistence in soil were studied in the field. A procedure was used which permited the analysis of residues of Chlorothalonil (DACONIL 2787) in sesame(Sesamum indicum L.)and soil. The procedure was based on the multiresidue analytical method using an polarized acetonitrile solution or acidified acetone as the extracting solvent. The DACONIL 2787 is separated from the fat in the extracts by using an activated alumina and Florisil chromatogaphic column. Residues of DACONIL 2787 were determined by subjecting the alternate eluate from the Florisil column to gas chromatographic analysis(ECD). Residue of chlorothalonil in sesame are proved to 0.06 ppm for six sprays, 3rd day before harvest The half-life of chlorothalonil in soil proved to be 8.9 days and residues of chlorothalonil was only 0.03 ppm 100 days after application of 15 ppm.

• The Korean Journal of Pesticide Science
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• v.20 no.2
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• pp.104-127
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• 2016

A new analytical method has been developed to determine 320 pesticides in apple and rice. The extraction of pesticides was carried out based on QuEChERS sample extraction, and determination was performed using LC-MS/MS and GC-MS/MS. 320 pesticides were selected for experiments. 251 and 110 pesticides among them were analysed by LC-MS/MS and GC-MS/MS, respectively. 41 pesticides of them were analyzed by both GC-MS/MS and LC-MS/MS. Among pesticides analysed by LC, 242 pesticides (96% of total number) in apple and 237 pesticides (94% of total number) in rice showed recoveries in the range of 70~120% with RSD ${\leq}20%$. In case of pesticides analyzed by GC-MS/MS, 103 pesticides (94% of total number) in apple and 83 pesticides (76% of total number) in rice were successfully validated. These results indicated that LC-MS/MS and GC-MS/MS analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in agricultural products.

• The Korean Journal of Pesticide Science
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• v.15 no.3
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• pp.238-245
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• 2011

This study was carried out to examine residual pesticides in dried agricultural products collected from Gyeonggi province in 2010. A total of 102 samples was collected and analyzed for 206 pesticides by multiresidue method using GC-${\mu}ECD$, GC-NPD, GC/TOF/MSD, HPLC-UVD, HPLC-FLD and HPLC/MS/MS. The detection rate of residual pesticides was 23.5% (24 of 102 samples) and the agricultural products exceeding their MRLs (Maximum Residue Limits) were 1 sample of pepper leaves. Additionally, the frequently detected pesticide were chlorothalonil, fenvalerate, chlorpyrifos, endosulfan, bifenthrin, cypermethrin, hexaconazole and iprodione. The pesticide types detected in the dried agricultural products showed in the descending order of organophosphorus (22%), pyrethroid (22%), organochloride (17%), dicarboxymide (11%), carboxymide (6%), carbamate (6%), triazole (5%) and the others (11%).

• The Korean Journal of Pesticide Science
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• v.16 no.4
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• pp.308-314
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• 2012

In order to monitor the residual pesticides in environment friendly agricultural commodities, fruits and fruiting vegetables. Twenty-five agricultural commodities were collected twice in May and August 2011 from nine environment friendly agricultural commodities-selling supermarkets and retail stores located in eight major cities in Korea. The number of each agricultural commodity collected, 555 samples in total, was 152 organic agricultural products, 202 pesticide-free agricultural products and 201 low-pesticide agricultural products. Pesticide residues in samples were analyzed by multiresidue method for 245 pesticides using a GC-ECD/NPD and an HPLC-DAD/FLD and the peaks suspected as pesticides were identified with a GC/MSD. As a result of pesticide residue analysis, three pesticides, bifenthrin, EPN and chlorpyrifos, were detected from four samples including apple, representing a detection rate of 0.72%. The residue levels of the four pesticide-detected samples were less than their maximum residue limits (MRLs) but one pesticide EPN detected from pear exceeded its legible criterion of one twentieth MRL. Estimated daily intakes of the pesticides detected from fruits and fruiting vegetables were less than 0.76% of their maximum permissible intake.

• The Korean Journal of Pesticide Science
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• v.14 no.1
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• pp.1-9
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• 2010

In order to survey residual characteristics of pesticides in the agricultural products selling at markets and to assess their safety, a total of 120 agricultural products were collected from the wholesale and traditional markets in Cheongju and analyzed the pesticide residues in them by multiresidue analysis method using GLC, HPLC and GC-MSD. Three pesticides, procymidone, penconazole, and tetraconazole, were detected from 4 samples such as onion, leek, tomato, and green pepper. Fungicide penconazole was detected from the onion collected from wholesale market. Fungicide procymidone was detected from leek and tomato and fungicide tetraconazole was detected from green pepper. Pesticide residues were detected from 3.3% of the total samples. The estimated daily intakes (EDIs) of the pesticides detected were less than 0.1% of their acceptable daily intakes (ADIs), representing that residue levels of the pesticides detected were evaluated as safe.

• Journal of Food Hygiene and Safety
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• v.35 no.5
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• pp.447-451
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• 2020

For this study, we conducted a simultaneous multiresidue analysis of veterinary drugs in cultured fishery products in Chungnam Province in 2018. A total of 115 fishery product samples were obtained from fish farms and fishery production sites located in the province. In all, 29 residual veterinary drugs in the samples were analyzed using a validated liquid chromatography-tandem mass spectrometry (LC-MS/MS) method. As a result, veterinary drug residues were only detected in a small number of the 106 samples (92.2%), and the detection rate was 7.8% (9 of 115 samples). The amounts were also below maximum residual limit (MRL) for fishery products, although one sample exceeded the MRL allowed by the Ministry of Food and Drug Safety and was detected in loach. The nine residual veterinary drugs were detected in 8 samples: loach, eel, catfish, freshwater bream, flatfish, rockfish and shrimp. The detected veterinary drugs were oxolinic acid, enrofloxacin, ciprofloxacin, sulfadiazine, flumequine and oxytetracycline. The most frequently detected antibiotic was oxolinic acid, and enrofloxacin exceeded the MRL in loach sample. Residues of most veterinary drugs were either not detected or were below the MRL, and while the status of fishery products is seen as safe overall, current surveillance efforts over veterinary drugs should be continued.

• Korean Journal of Environmental Agriculture
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• v.12 no.3
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• pp.239-246
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• 1993

In order to clarify the possible contamination of rice straw used as a crude feed for livestock, Korean native cattle and cow, by pesticides, the samples collected from 21 sites in Korea were analyzed by a multiresidue method for 10 pesticides with GLC to obtain the following results. 1. Detection limits were 0.001ppm in butachlor, 0.002ppm in chlorpyrifos, 0.003ppm in BPMC, pirimiphos-methyl and diazinon, 0.004ppm in fenitrothion, 0.005ppm in phenthoate, 0.009ppm in IBP, 0.015ppm in carbofuran, and 0.03ppm in carbaryl. 2. In recovery tests, 73-101% of the pesticides applied were recovered, the recovery being low in carbofuran and chlorpyrifos. 3. Butachlor, 2-chloroacetanilide herbicide, and BPMC, carbaryl, and carbofuran, carbamate insecticides, were not detected in any sample. 4. In organophosphorus insecticides, the amounts of fenitrothion in sample No. 1, 2, 4, 5, 7, 12, 20 and 21 were in the range of 0.01-0.05ppm, those of phenthoate detected in sample No. 10 and 12 were 0.4 and 0.17ppm, respectively, and those of IBP in all samples, with the exception of sample No. 7, 12, 16, 17, 20, and 21, were in the range of 0.01-0.20ppm. The residues of chlorpyrifos, diazinon, and pirimiphos-methyl were not detected.