• Korean Journal of Veterinary Service
• /
• v.28 no.3
• /
• pp.203-213
• /
• 2005

Oxytetracycline, tetracycline, chlortetracycline and doxycycline in honey were separated by solid phase extraction (SPE) and determined with high performance liquid chromatography (HPLC) with UV/Visible detector. Analysis was carried out using following conditions: XTerra $C_8$ column $(3.9\times150mm\;i.d. 5{\mu}m)$, mobile phase composed of 0.01M oxalic acid : methanol : acetonitrile (820 : 80 : 100, v/v/v), isocratic pump at a flow rate of 0.9 ml/min. and $50{\mu}l$ of injection volume, UV/Visible detector with wavelength of 360nm. The calibration curves of four tetracyclines showed linearity $(\gamma^2>0.999)$ at concentration range of $100\~1,000 ng/ml$. The recoveries in fortified honey represented more than $70\%$ with low coefficient of variation $(<10\%)$ for concentration range of four tetracyclines. The detection limits for oxytetracycline, tetracycline, chlortetracycline and doxycycline were 13.8, 14.6, 26.2 and 24.9ng/g in acacia honey. respectively. We also monitored tetracyclines residue in domestic honey [n : 38, acacia (20), wild flower (18) ] and foreign honey [n=22, legally distributed (13), illegally distributed (9)] using modified Charm II screening and HPLC confirmation methods. Seven of the 60 samples $(11.7\%)$ were suspect positive using modified Charm II screening test. Chlortetracycline residue was found in one foreign honey (illegally distributed) tested at concentrations of 0.22 ppm. Conclusively, for more effective control of tetracyclines used in beekeeping should be further survey for residues in honey and also national guidelines (maximum residue limit : MRL) and methods should be obligatory.

• Korean Journal of Environmental Agriculture
• /
• v.38 no.4
• /
• pp.321-331
• /
• 2019

BACKGROUND: Pinoxaden is the phenylpyrazoline herbicide developed by Syngenta Crop Protection, Inc. and marketed on 2006. The maximum residue levels for wheat and barley were set by import tolerance. Thus, Ministry of Food and Drug Safety (MFDS) official analytical method determining Pinoxaden residue was necessary in various food matrixes. Satisfaction of international guideline of CODEX (Codex Alimentarius Commission CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) are additional pre-requirements for analytical method. In this study, liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was investigated to analyze residue of Pinoxaden (M4), which is defined as pesticide residue in Korea, in foods. METHODS AND RESULTS: Pinoxaden (M4) was extracted followed by acid digestion (2hr reflux with 1N HCl) and pH adjusting (pH 4-5 with 3% ammonium solution). To remove oil, additional clean-up step with hexane saturated with acetonitrile was required to high oil contained sample before purification. HLB cartridge and nylon syringe filter were used for purification. Then, samples were analyzed by LC-MS/MS using reserve phase column C₁₈. Five agricultural group representative commodities (mandarin, potato, soybean, hulled rice, and red pepper) were used to verify the method in this study. The liner matrix-matched calibration curves were confirmed with coefficient of determination (r²) > 0.99 at calibration range 0.002-0.2 mg/kg. The limits of detection and quantitation were 0.004 and 0.01 mg/kg, respectively, which were suitable to apply Positive List System (PLS). Mean average accuracies of pinoxaden (M4) were shown to be 74.0-105.7%. The precision of pinoxaden and its metabolites were also shown less than 14.5% for all five samples. CONCLUSION: The method investigated in this study was suitable to CODEX (CAC/GL 40) and National Institute of Food and Drug Safety Evaluation-MFDS (2017) guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

• The Korean Journal of Pesticide Science
• /
• v.18 no.2
• /
• pp.61-68
• /
• 2014

Dissipation constants and half-lives of acaricides etoxazole and flufenoxuron in apples were calculated to establish their pre-harvest residue limits (PHRLs). The acaricides were sprayed on apples with single and triple doses based on safe use guidelines, and their residual patterns in the apple were interpreted using first order kinetics equation. The residual amounts of acaricides during the experimental period were below their maximum residue limits (MRL) for apple. The dissipation constants of acaricides in the apples were calculated at 0.0788 for etoxazole and 0.0319 for flufenoxuron corresponding to their biological half-lives; 8.8~21.7 days for etoxazole and 21.7~23.1 days for flufenoxuron. The PHRLs of acaricides in the apple showed the residual amounts of etoxazole and flufenoxuron at the harvesting date would be below their MRLs if their residual amounts were less than 0.87 and 0.88 mg/kg, respectively, at 7 days prior to harvesting the apples.

• The Korean Journal of Food And Nutrition
• /
• v.14 no.5
• /
• pp.446-456
• /
• 2001

This study was carried out for the dietry safely based on the level of pesticide residues In 13 kinds of agricultural products consumed in Kyonggi-Do. Korea. From June to October 2000, sixteen organochlorine pesticides in 397 samples were analyzed by using GC/ECD and GC/MSD. According to the results, endosulfan were detected in 27(7.8%) samples and chlorothalonil were detected in 4(1.0%) samples. Detection ranges of endosulfan were 3.7437∼ 0.0488ppm for lettuce, 2.1902 ∼0.1423ppm for spinach, 2.4909 ∼0.0786ppm for mallow and 3.2333∼0.3997ppm for mustard leaf, respectively Chlorothalonil were 5.8097 for lettuce and 0.8962ppm for spinach. Consequently, six agricutural products were detected more than the maximum residue limits in Korea Endosulfan were detected In 5(1.8%) samples and cholrothalonil were detected in 1(0.3%) sample. Detection rates of endosulfan sulfate(45.9%) of agricultural products were more than $\alpha$-endosulfan(28.5% ) and $\beta$-endosulfan (23.9% ) .

• The Korean Journal of Pesticide Science
• /
• v.10 no.4
• /
• pp.266-271
• /
• 2006

This study was monitored for 14 pesticide residues in agricultural products for the army, such as fruit vegetables(pepper, cucumber, pumpkin, melon and water melon), leafy vegetables(Korean cabbage, spinach, lettuce, crown daisy, cabbage, green onion), mushrooms(agaric, p'yogo), and bean sprouts produced in Kyunggi-do and Inchon-City. From January to December 2005, ten carbamate pesticides in 356 samples were analyzed by HPLC. One kind of pesticide was detected in 8 samples of detection rate (2.53%), and two pesticides were in one sample of detection rate(0.27%). Aldicarb, bendiocarb, fenobucarb, methiocarb, isoprocarb, and propoxur were not found in all samples. Detection rates of pesticides were 0.84% for methomyl, 0.56% for carbofuran, 0.56% for ethiofencarb, and 0.28% for carbayl. Dectection ranges of pesticides were from 0.01 to 2.9 mg/kg for ethiofencarb, from 0.1 to 0.23 mg/kg for methomyl, from 0.20 to 0.24 mg/kg for carbofuran, and 0.01 mg/kg for carbaryl, respectively. Consequently, detection levels of all pesticides in samples were less than the maximum residue limits(MRLs) in Korea representing that all agricultural products for the army were safe.

• The Korean Journal of Pesticide Science
• /
• v.19 no.2
• /
• pp.81-87
• /
• 2015

The present study was aimed to predict the pre-harvest residue limits (PHRLs) of pyrimethanil (fungicide) and methoxyfenozide (insecticide) in grape, and to estimate their biological half-lives and residual characteristics. The pesticides were sprayed once on grape in two different fields 10 days before harvest. At the end of 0, 1, 2, 3, 5, 7 and 10 days after application, samples were harvested for further analysis. The residual pesticides were extracted with acetonitrile and partitioned with dichloromethane, and the high-performance liquid chromatography with diode array detector (HPLC/DAD) was employed for the residue analysis. The results obtained in the present study show that the limit of detection of both pesticides were found to be $0.01mg\;kg^{-1}$. The recoveries of these pesticides were ranged between 80.6% and 102.5% with coefficient of variation lower than 10%. The biological half-lives of both pesticides were observed in field 1 and field 2 which shows 7.7 and 7.4 days for pyrimethanil and 5.1 and 6.1 days for methoxyfenozide, respectively. Further, the PHRL of pyrimethanil and methoxyfenozide was found to be $8.90mg\;kg^{-1}$ and $5.51mg\;kg^{-1}$, respectively at 10 days before harvest. Consequently, the present study suggests that the residual amounts of both pesticides will be lower than the maximum residue limits (MRLs) when grape is harvested.

• Journal of Food Hygiene and Safety
• /
• v.14 no.2
• /
• pp.201-215
• /
• 1999

Limited information is available on the acceptability of Korean MRLs(maximum residue limits) and the health risk based on the pesticide exposure by food intake. The aim of this study was to evaluate TMDI(theoretical maximum daily intake) and EDI(estimated daily intake) for Korean by using MRLs, food intake, residue data, and correction factors, and compare with ADI(acceptable daily intake) in order to estimate the health risk based on the pesticide exposure. The study was performed in three steps. In the frist step, the residual pesticides in each category of food were investigated using the pesticide residue analytical data(1995-96) from officially approved organizations and the analytical data for poultry was adopted from Korean food code method. In the second step, TMDI was estimated from MRLs and food factors, and was compared with ADI. In the third step, the effectiveness of each culinary treatment (washing, peeling, steaming, boiling, and salting) was evaluated and EDI was calculated using pesticide residue data, food factor, and correction factor by treatment. TMDI obtained from MRLs and food intake, and food intake was summed as 1,100.99 g, which was 79.1% of total consumption. The percent ratio of TMDI to ADI for 156 pesticides was mostly below 80% and only 30 pesticides exceeded the ADI. In particular, non-treated EDI from pesticide residue data and food intake was summed up to about 43 $\mu\textrm{g}$/day/capita, and the rank was procymidone(8.6 $\mu\textrm{g}$) > maleic hydrazide(8.2 $\mu\textrm{g}$) > EPN(3.7 $\mu\textrm{g}$) > deltamethrin(3.5 $\mu\textrm{g}$) > cypermethrin(3.0 $\mu\textrm{g}$). The treated EDI calculated from pesticide residue data, food intake, and correction factor by culinary treatment was summed up to 13.7 $\mu\textrm{g}$/day/captia. The percentage of ADI was TMDI(79.74%) > non-treated EDI (0.17%) > treated EDI (0.04%), and the exposure level of Korean population to whole pesticides was below the level to produce health risk. Oncogenic risk of five pesticides used in Korea whose oncogenic potency(Q*) was known were assessed from TMDI and treated EDI. Dietary oncogenic risk for Korean was estimated to be 2.0$\times$10-3 on the basis of TMDI, 8.3$\times$10-7 on the basis of treated EDI. The oncogenic risk from TMDI exceeded the risk level(1$\times$10-6) of EPA, whereas the oncogenic risk from treated EDI and real exposure level lower than that of EPA.

• Journal of fish pathology
• /
• v.27 no.1
• /
• pp.67-75
• /
• 2014

Aquaculture drugs have used to prevent disease in aquaculture field for many years. In spite of many advantages, overdose and abuse may cause environmental pollutions and antibiotic resistances. Many countries try to protect the environment, biospecies and food safety. Recently, Korea enact laws and ordinances such as the Aquatic Animal Disease Control Act. The purpose of this act to contribute to the stable production and control system for aquatic diseases. The Maximum residue limits (MRLs) of aquaculture drugs have been established by Ministry of Food and Drug Safety (MFDS) and Drug licensing was in National Fisheries Research and Development Institute (NFRDI) by Aquatic Animal Disease Control Act. There is 750 items in aquaculture drugs and these are classified into 4 group, which is approval, necessary for prescription, unregulated and safety drug, and banned drug. MRLs of 30 items in aquaculture drug have been established by Food Sanitation Act. Future research is required to determine the suitable for abundant varied fishes of drugs for side effects and safety.

• Korean Journal of Environmental Agriculture
• /
• v.23 no.4
• /
• pp.251-257
• /
• 2004

Analytical methods were developed to determine cyclosulfamuron residues in soil, water, rice grain and straw using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. In these methods, cyclosulfamuron was extracted with aqueous $Na_2HPO_4$/acetone and acetone/methanol mixture from soil and rice samples respectively. Liquid-liquid partition coupled with ion-associated technique, Florisil column chromatography, and solid-phase extraction (SPE) were used to separate cyclosulfamuron from interfering co-extractives prior to HPLC analysis. For water sample, the residue was enriched in $C_{18}$-SPE cartridge, cleaned up in situ, and directly subjected to HPLC. Reverse-phase HPLC under ion-suppression was successfully applied to determine cyclo-sulfamuron in sample extracts with the detection at its ${\lambda}_{max}$ (254 nm). Recoveries from fortified samples averaged $87.8{\pm}7.1%$ (n=12), $97.3{\pm}7.2%$ (n=12), $90.8{\pm}6.6%$ (n=6), and $78.5{\pm}6.7%$ (n=6) for soil, water, rice grain and straw, respectively. Detection limits of the methods were 0.004 mg/kg, 0.001 mg/L, 0.01 mg/kg and 0.02 mg/kg for soil, water, rice grain and straw samples, respectively.

• The Korean Journal of Pesticide Science
• /
• v.17 no.3
• /
• pp.155-161
• /
• 2013

The residue patterns of clothianidin and thiacloprid, insecticides registered in the ginseng, were investigated to predict pre-harvest residues limits (PHRL). Pesticides were treated under Korea GAP (Good Agricultural Practices) with the recommended dose (single dose) and twice of recommended dose (double dose). Samples were collected 11 times over 42 days (each 0, 2, 5, 8, 12, 16, 20, 24, 28, 33, 42 days after treatment). Residues of clothinidin and thiacloprid were analyzed by UPLC/TQD. Biological half-life of clothinidin in single dose and double dose were 14.6 days and 10.2 days and that of thiacloprid were also 9.7 days and 11.2 days, respectively. The PHRL of ginseng on 10 days before harvest was 0.3 mg/kg in clothianidin and 0.18 mg/kg in thiacloprid.