This study was carried out to survey the residual characteristics of pesticides and assess their safety. Nineteen agricultural commodities, collected from wholesale and traditional markets in Cheongju. Nineteen agricultural commodities including perilla leaves were collected from the markets on October 29th, 2010. Total 240 pesticides which can be analyzed by multiresidue analysis method by GLC and HPLC were monitored and the pesticides detected were confirmed by GC-MSD and LC-MS. Five pesticides, alachlor, bifenthrin, endosulfan, procymidone and triflumizole, were detected from five samples, such as welsh onion, leek and celery in case of wholesale market and perilla leaves and welsh onion in case of traditional market. Detection rate of 13.2% was obtained as a result of pesticide analysis but 2.6% of the pesticides detected exceeded their maximum residue limits. The estimated daily intakes (EDIs) and maximum permissible intakes (MPIs) of the pesticides detected were less than 26% and 0.05% of their acceptable daily intakes (ADIs) respectively, representing that residue levels of the pesticides detected would be safe.
The aim of this study was to develop an analytical method for the quantification of diazepam residues in fishery products, using liquid and gas chromatography-tandem mass spectrometry (LC-MS/MS and GC-MS/MS). The sample utilized in the study was extracted from the fish sample (crucian carp) using 0.1% formic acid in acetonitrile. For the utilization of the purification process, the dispersive solid phase extraction (dSPE) was used for LC-MS/MS, dSPE and SPE was used for GC-MS/MS, respectively. To be sure, the standard calibration curves showed a good linearity as the noted correlation coefficients, $r^2$ was > 0.99. The average recoveries for accuracy ranged in 99.8~124% for the samples which were fortified at three different levels (0.001, 0.002 and 0.010 mg/kg). The correlation coefficient for the precision effect was measured at a range of 4.01~11.8%. The limit of detection (LOD) for the diazepam analysis was 0.0004 mg/kg, and the limit of the quantification (LOQ) was 0.001 mg/kg. The proposed analytical method was characterized with a high accuracy and acceptable sensitivity to meet the established Codex Alimentarius Commission (CAC/GL71-2009) guideline requirements. We therefore established the optimal analysis method for the determination of diazepam in the fishery products using LC-MS/MS and GC-MS/MS. It would be applicable to analyze the diazepam residues in fishery products in further studies on this subject.
Pesticide has played important role in Korean and Austrailian agriculture. In addition, pesticides are the most reliable tools pests in agriculture. Recently, it is highly recommended that the use of pesticide should be concerned with both atricultural and environmental aspect, also legislation on environmental contamination has been fortified to the world. Particularly, the attention on agrochemicals has been focused on the soil abuse and the water contamination at present time. In spite of this kind of concern, a few research about pesticides using in Australia and Korean have been conducted to their behaviors under australian and korean environment to avoid environmental contamination by pesticides. Thus, the research organizations need facilities to analyze the characteristics of each pesticide and the environmental fate of pesticides. The conventional analytical method to detect pesticides and their metabolites can not be overcome to reduce time, expenditure, and complexity of analysis even though the methods are accurate and precise. For example, High performance liquid chromatography(HPLC), and gas chromatography (GC) used until now are less choice detectors and often lower sensitive. In contrast to the conventional analytical methods, biosensors are so fast in analysis and has high productivity and analyze multi=sample simultaneously. Therefore, it is biosensing analytical method that we could consider as an alternative method intead of the conventional methods.
Kim, Tae Hee;Jang, Seol;Lee, Ah Reum;Lee, A Young;Choi, Goya;Kim, Ho Kyung
The Korea Journal of Herbology
/
v.27
no.6
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pp.43-48
/
2012
Objectives : This study was investigated to determine the contents of pesticide residues and sulfur dioxide residues in commercial herbal medicines in Korea. Methods : Chromatographic test was performed on 100 samples consisted with 10 kinds of medicinal plants including improted and domestic products. To establish 19 pesticide residues (DDE, DDD, DDT, Dieldrin, Methoxychlor, BHC isomers, Aldrin, Endosulfan isomers, Endrin, Captan, Procymidone, Chlorpyrifos and Imidacloprid) in commercial herbal medicines, chromatographic equipments were used with the gas chromatography-mass detector and gas chromatography-electron capture detector for qualitative analysis. The imidacloprid analysis was performed by high performance liquid chromatograpgy-ultraviolet detector at 270 nm UV wavelength. The contents of sulfur dioxides were analyzed by modified Monnier-Williams method. All methods were based on notification procedure of Korea Food & Drug Administration (KFDA). Results : The residual pesticides were not founded in improted and domestic samples. Among 100 samples, the residues of sulfur dioxide in 73 samples were not detected and 25 samples showed contents in the range of 0~21.90 mg/kg. The excess samples of MRLs were 2 samples (30 mg/kg to medicinal herbs), Asiasari Radix et Rhizoma (Imported product) and the average amount of sulfur dioxide in 2 unsuitable samples were 14.83 mg/kg. These samples were found to transgress KFDA regulatory guidance of residual sulfur dioxide. Conclusion : These results are able to use as basic data to improve the reliability and value of commercial medicinal herbs.
A simultaneous analytical method was developed for the determination of isoxaflutole and metabolite (diketonitrile) in agricultural commodities. Samples were extracted with 0.1% acetic acid in water/acetonitrile (2/8, v/v) and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2 by 1 N hydrochloric acid. The analytes were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive-ion mode using multiple reaction monitoring (MRM). Matrix matched calibration curves were linear over the calibration ranges ($0.02-2.0{\mu}g/mL$) for all the analytes into blank extract with $r^2$ > 0.997. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries were ranged between 72.9 to 107.3%, with relative standard deviations (RSDs) less than 10% for all analytes. All values were consistent with the criteria ranges requested in the Codex guideline (CAC/GL40, 2003). Furthermore, inter-laboratory study was conducted to validate the method. The proposed analytical method was accurate, effective, and sensitive for isoxaflutole and diketonitrile determination in agricultural commodities.
Journal of agricultural medicine and community health
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v.28
no.1
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pp.29-37
/
2003
Objectives: This study was performed to evaluate the pesticide exposure status and acute pesticide poisoning symtoms among agricultural workers at Gangwon-do province alpine area. Alpine area was defined as the area higher than 400m. Methods: We analyzed 257 interviwed questionnaire about pesticide exposure, acute pesticide poisoning symptoms and other variables. Results: The result was shown that agricultural workers at alpine area used more pesticide than general agricultural workers for annual usage days(35.9 days vs 14.4 days), daily usage hours(6.7 hrs vs 2.8hrs, p<0.05). But there was no difference between general and alpine agricultural worker's herbicide exposure. Moreover, the alpine agricultural worker's acute pesticide poisoning symtom score was higher than general agricultural worker's. These difference was also found at result of regression analysis, under control the age, sex, monthly income. Most frequently suffered symptom was headache and dermatological problems. The symptom prevalence of dermatological problem, headache, general weakness, eye irritation, nausea were higher among alpine agricultural workers than general agricultural workers. Conclusions: As a result, agricultural workers at alpine area were more exposed to pesticide and suffered from pesticide poisoning symptoms. To prevent the symptoms and disease from pesticide exposure among agricultural workers at alpine area, more research and political effort will be needed.
The objective of this study was to develop a simultaneous method of 8 penicillin antibiotics including amoxicillin, ampicillin, cloxacillin, dicloxacillin, nafcillin, oxacillin, penicillin G and penicillin V in meat using LC-MS/MS. The procedure involves solid phase extraction with HLB cartridge and subsequent analysis by LC-MS/MS. To optimize MS analytical condition of 8 compounds, each parameter was established by multiple reaction monitoring in positive ion mode. The chromatographic separation was achieved on a $C_{18}$ column with a mobile phase of 0.05% formic acid and 0.05% formic acid in acetonitrile at a flow rate of 0.2 mL/min for 20 min with a gradient elution. The developed method was validated for specificity, linearity, accuracy and precision in beef, pork and chicken. The recoveries were 71.0~106%, and relative standard deviations (RSD) were 4.0~11.2%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.003~0.008 mg/kg and 0.01~0.03 mg/kg, respectively, that are below maximum residue limit (MRL) of the penicillins. This study also performed survey of residual penicillin antibiotics for 193 samples of beef, pork and chicken collected from 9 cities in Korea. Penicillins were not found in all the samples except a sample of pork which contained cloxacillin (concentration of 0.08 mg/kg) below the MRL (0.3 mg/kg).
The effects of feeding Brassica vegetable market wastes on intake, body weight changes and pesticide/insecticide residues in products of goats were evaluated in two experiments. In the first experiment (Exp. 1) 16 goats (Bach Thao, 9 to 10 kg, 3 months old, 9 males and 7 females) were fed four diets with leaves either from cabbage (Brassica oleracea var. capitata), cauliflower (Brassica oleracea var. botrytis) or Chinese cabbage (Brassica campestris subsp. pekinensis) with 30% of Para grass. The control group was fed 100% Para grass. All diets contained soybean waste as a supplement and the experiment lasted for 136 days. In the second experiment (Exp. 2) 24 goats (Bach Thao, 12 to 14 kg, all males) were assigned to three treatments in a completely randomised block design based on initial body weight. The goats were fed cabbage waste supplemented with 200 g or 100 g DM (dry matter) of concentrate. Para grass with 100 g DM concentrate supplementation was used as a control group. The experiment lasted for 90 days and at the end of the study, 12 goats were slaughtered for pesticide/insecticide analysis. Due to low DM content (5.3 and 3.7%, respectively) feed intakes of cabbage and Chinese cabbage groups were lower than those of other groups in the experiment. The highest feed intake and body weight gain was obtained when the goats were fed cauliflower (529 g DM/day and 87.5 g/day, respectively). In Exp. 2 total intake of cabbage and concentrate was similar (484 g and 453 g DM/day) whether the goats were fed 100 or 200 g concentrate/day but lower than that of Para grass and concentrate probably due to the low DM content of the cabbage (5.9%). Crude protein intake (79 g to 86 g/day) and body weight gain (70 g to 88 g/day) was not significantly different between treatments. Adding concentrate consequently resulted in higher DM intake than in Exp. 1 but did not result in any higher growth rate. Three of the pesticide/insecticide residues tested were found in cabbage, Alpha-Cypermethrin, Bassa-Fenobucarb and Dimethoate with levels of 0.175, 0.074 and 0.028 mg/kg fresh cabbage respectively. Weight of livers from goats fed cabbage was about 90 g higher than from goats fed Para grass but no pesticide/herbicide residues were found in meat or liver.
Cyantraniliprole, which is an ananthranilic diamide insecticide that was developed by the DuPont Corporation, was registered in the Republic of Korea in 2012. It offers exceptional insecticidal activity on a broad range of Lepidopera, Coleoptera, Diptera, and Isoptera. The maximum residue limits are set to pepper, peach, apple, sweet pepper, welsh onion, and so on (0.2~2.0 mg/kg). Therefore, an analytical method for determining cyantraniliprole residue in agricultural products was developed to ensure food safety. In previous studies, welsh onions were among vegetables included in the allium species, which is a representative plant with sulfur organic compounds. In this study, the analytical method was developed and evaluated for the elimination of sulfur compounds from the test solution of allium species during pesticide residue analysis. In order to inactivate the enzyme allinase and produce sulfur compounds, sample extraction was made in the base state pH 10 by reducing the activity of the enzyme. The recoveries of the developed method ranged from 81.9% to 83.2%, and the relative standard deviations were less than 10%. Therefore, based on the results, the method developed in this study is accurate and appropriate for use in cyantraniliprole determination. It will be used as the official method for managing the safety of cyantraniliprole residues in agricultural products.
Journal of the Korea Academia-Industrial cooperation Society
/
v.21
no.10
/
pp.137-143
/
2020
To ensure safety of raw materials for military foods, hazard assessment and monitoring of residual pesticides was conducted on agricultural products consumed by 9 companies based in Gyeongin and Gangwon. Residual pesticides were analyzed for 142 different products, by applying the multi-species pesticide polycomponent analysis method. Of the 36 samples analyzed, residual pesticides were detected in 7 samples, representing a detection rate of 19.4%. One particular pesticide residue was detected in peanuts, green onions, and red pepper powder, and 20 types of pesticide residues were detected in red pepper powder used in combat foods. However, all residues were found to be below the permissible level. Moreover, the hazard assessment results for Cypermethrin, Tebuconazole and EPN showed the highest concentration among the residual pesticides detected. Since the estimated intake was less than 100% as compared to the ingestion limit, it was considered to be safe. I have suggested the edit as per my understanding. Please review for accuracy, and revise appropriately if required. This is the first pesticide Risk Assessment study encompassing military requirements. Considering the results, we expect further application research, including research on reducing hazardous materials.
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