• Title/Summary/Keyword: multi-pesticide analysis

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Simultaneous Determination of Pesticide Residues in Soils by Dichloromethane Partition - Adsorption Chromatography - GC-ECD/NPD Analytical Methods (Dichloromethane 분배 - 흡착 크로마토그래피 - GC-ECD/NPD 분석법에 의한 토양잔류농약 다성분 분석)

  • Kim, Chan-Sub;Lee, Byung-Moo;Park, Kyung-Hun;Park, Byung-Jun;Park, Jae-Eup;Lee, Young-Deuk
    • The Korean Journal of Pesticide Science
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    • v.14 no.4
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    • pp.361-370
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    • 2010
  • Considering the efficiencies of the preparation process at each stage obtained in previous studies, the analytical determination method was established for multi-pesticide residues in soils. It consist of the acetone-extraction, the dichloromethane-partition, the Florisil or silica-gel chromatography and the gas chromatography analysis equipped with the electron capture detector and the nitrogen-phosphorus detector. In the soil recovery test by Florisil clean-up system, the number of pesticides recovered in the range of 70~120% and showed less than 20% of RSD were 165 pesticides for paddy soil, 169 pesticides for upland soil and 159 pesticides in both soils through the tested 183 pesticides. And in the soil recovery test by silica-gel system, the number of pesticides recovered in the range of 70~120% and showed less than 20% of RSD were 154 pesticides for paddy soil, 145 pesticides for upland soil, and 134 pesticides in both soils.

Susceptibility of Spodoptera exigua to UVA Insecticides Using Agricultural Multi-copter on Cabbage Field (농업용 멀티콥터를 활용한 무인항공기용 작물보호제에 대한 배추 파밤나방의 약제감수성)

  • Park, Bueyong;Lee, Sang-Ku;Jeong, In-Hong;Park, Se-Keun;Lee, Sang-Bum;Kim, Gil-Hah
    • Korean journal of applied entomology
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    • v.58 no.4
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    • pp.271-280
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    • 2019
  • We investigated the control efficacy and phytotoxicity of unmanned aerial vehicle-applied pesticides against the insect Spodoptera exigua, a major emerging pest in Chinese cabbage. Phytotoxicity was investigated in cabbage and 7 crops cultivated in the perconducted on 8 surrounding crops including Chinese cabbage at 1 to 2 times the recommended pesticide dosage. We treated cabbage fields with spinetoram suspension concentrate (16×), methoxyfenozide, sulfoxaflor suspension concentrate (16×). Then, we used water-sensitive paper to measure the distribution pattern of falling pesticide particles and the degree of coverage. Two of the pesticides showed 97% control efficacy, however, control efficacy might differ in resistant populations. Phytotoxicity was not observed in Chinese cabbage and the 7 surrounding crops treated with 1 to 2 times the recommended pesticide dosage. Analysis of the distribution pattern of falling pesticide particles revealed that breeze caused particle diffusion. Thus, wind is an important factor affecting the uniform treatment and diffusion of multicopter-applied pesticides. It follows that setting optimal conditions is necessary for effective control and treatment.

Efficiency of Silver Ion-Silica Solid Phase Extraction for Elimination of Sulfur Compounds during Pesticide Multiresidue Analysis in Allium Species (파속류의 잔류농약분석과정에서 silver ion-silica solid phase extraction에 의한 황화합물의 제거 효율성)

  • Park, Jin-Woo;Moon, Kyung-Mi;Choi, Young-Whan;Lee, Young-Guen
    • 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%.

Development of Analytical Reference Material for Proficiency Test of Pesticide Multi-residue Analysis in Green-pepper (풋고추 농약다성분분석 정도관리용 분석표준물질 개발)

  • Kim, Jong-Hwan;Choi, Sung-Gil;Oh, Young-Gon;Kwon, Young-Sang;Hong, Su-Myeong;Sung, Mun-Hyun;Lee, Se-Ja;Hwang, Sun-Young;Seo, Jong-Su
    • The Korean Journal of Pesticide Science
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    • v.20 no.3
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    • pp.211-220
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    • 2016
  • This study was to develop the analytical reference material of green-pepper for multi-residue analysis of pesticides. According to the ISO Guide 35, ISO Guide 13528 and EURL-PT protocol, the homogeneity, stability, assigned value and uncertainty were calculated to assess if it was suitable to be used as the proficiency test or quality control. The values of the within-bottle standard variation ($s_{wb}$) and the between-bottle standard variation ($s_{bb}$) were 1.7~3.7% of assigned value according to the requirement of the ISO guide 35. And, the uncertainty ($u^*{_{bb}}$) due to inhomogeneity was 0.8~1.1% for all pesticides. The storage stabilities of ten-pesticides at various conditions were assessed. For all target pesticides, the slop ($b_1$) values were smaller than the corresponding values of $[t_{0.95,n-2}{\times}s(b_1)]$ specified by the ISO guide 35, indicating that there were no statistically significant decreases in the concentration of the target pesticides when the analytical reference material was stored at room temperature ($20{\sim}30^{\circ}C$) for 7 days, freezing ($-20^{\circ}C$) for 30 days and deep freezer ($-80^{\circ}C$. except for bifenthrin, fenpropathrin) for 245 days. For proficiency test by using it developed by Korea Institute of Toxicology, inter-lab test was performed with eight organization performing the residual pesticide analysis. We found that there were some different results among them. Some were assessed as questionable or unacceptable for two pesticides and one organization didn't analyze the six pesticides. From these results, this green-pepper analytical reference material containing ten-pesticides could be used as a tool for the proficiency test to improve the reliability or consistency for pesticide residue's results.

Environmental Impacts and Rapid Analysis by Biosensors of Agrochemicals in Korea and Australia (한국과 호주에서의 Biosensor 에 의한 농약의 환경영향 조기검출)

  • Lim, Soo-Kil;Kennedy, I.R.;Lee, Sung-Eun;Jeong, Chang-Yoon;Kim, Jeong-Gyu
    • Korean Journal of Environmental Agriculture
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    • v.17 no.4
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    • pp.371-378
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    • 1998
  • 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.

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Development of Analytical Method for Colistin in Fish and Shrimp using Liquid Chromatography Mass Spectrometry (LC-MS/MS를 이용한 수산물 중 콜리스틴 분석법 개발)

  • Shin, Dasom;Kang, Hui-Seung;Lee, Soo-Bin;Cho, Yoon-Jae;Cheon, So-Young;Jeong, Jiyoon;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.31 no.5
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    • pp.319-326
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    • 2016
  • Colistin is a last resort antimicrobial agent against multi-drug resistant Gram-negative bacteria. This study was conducted to develop an analytical method to determine colistin in fish and shrimp. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with acidified 5% methanol (containing 0.5% formic acid). Then, solid phase extraction (SPE) was used for cleanup. Matrix-matched calibration curves were linear over the calibration ranges (0.05-1.2 mg/kg) for all the analytes into blank sample with $r^2$ > 0.99. All the values fulfilled the criteria requested by the Codex guidelines. Average recoveries ranged from 85.9% to 107.9%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was less than 15%. The limit of detection (LOD) was 0.02 mg/kg, and the limit of quantitation (LOQ) was 0.05 mg/kg. This improved method showed higher accuracy and acceptable sensitivity to meet the CAC guideline requirements and is applicable for the analysis of residual colistin (A+B) in fish and shrimp.

Monitoring of Pesticide Residues and Risk Assessment of Agricultural Products Consumed in South Korea (국내유통농산물 중 잔류농약 모니터링 및 안전성 평가)

  • Kim, Sung-Hun;Choe, Won-Jo;Baik, Yong-Kyoo;Kim, Woo-Seong
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.37 no.11
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    • pp.1515-1522
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    • 2008
  • Monitoring the pesticide residues in agricultural products is essential to protect consumers, obtain data for risk assessment, and ensure fair trade practices. We developed a multi-residue method for the analysis of 37 pesticides with different physico-chemical properties in agricultural products and analyzed the amount of pesticide residues on about 1,000 samples circulated in South Korea. The samples consisted of 26 different types of agricultural products selected at markets in 14 major cities; cereals (2 species), nuts (1 species) potatoes (1 species), beans (2 species), fruits (3 species), vegetables (16 species), and mushrooms (1 species). In this study, residual pesticides were detected in 23 samples (2.2%) and one sample was detected to be over maximum residue limits (MRLs, 0.1%) for pesticides in foods by the Korea food code. In leafy vegetables such as pepper leaves, radish leaves, cham-na-mul, shin-sun-cho, crown daisy, chwi-na-mul and citrus fruits such as kumquat, 8 kinds of pesticides were detected. Specially, diazinon were detected over MRLs and also, endosulfan, ethoprophos and phenthoate were detected frequently. Based on these results, we investigated the risk assesment from amount of residual pesticide, total %ADI was 1.262%, but the value has not effected on human health.

Research of pesticide residue of domestic Lentinula edodes related with the positive list system (농약 허용물질목록 관리제도와 연계한 국내산 표고 잔류농약 실태 조사)

  • Kim, Kyung-Je;Koh, Young-Woo;Im, Seung-Bin;Jin, Seong-Woo;Ha, Neul-I;Jeong, Hee-Gyeong;Jeong, Sang-Wook;Yun, Kyeong-Won;Seo, Kyoung-Sun
    • Journal of Mushroom
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    • v.18 no.4
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    • pp.380-386
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    • 2020
  • The study was conducted for the safety evaluation of 320 pesticide residues in 768 Lentinula edodes fruit body samples and 143 L. edodes media samples, which are distributed nationwide in South Korea. The monitoring method was the second of the multi-residue methods in the Korean Food Code. GC-ECD, GC-NPD, and GC-MSD were used as evaluation equipment for analysis. Single-analysis of the target pesticides was performed for mepiquat chloride. Through the analysis of collected L. edodes samples, pesticide residues were detected in total seven cases, including four L. edodes fruit body samples and three L. edodes media samples. The detected pesticide residues were carbendazim, diflubenzuron, fluopyram, and dinotefuran. In this study, carbendazim was detected in three L. edodes fruit body samples and one L. edodes media sample. The detected amount of carbendazim was 0.056, 0.17, 0.043, and 0.09 mg/kg, respectively. The amount of carbendazim in the collected L. edodes samples was detected below the MRLs (maximum residue level). The detected amounts of fluopyram and dinotefuran were 0.068 mg/kg and 0.06 mg/kg, respectively. Two pesticide residues were detected in the medium in one case. Mepiquat chloride was not detected in this study. These results suggested that residual pesticides were detected in a small number of collected L. edodes. However, the PLS for unregistered pesticides MRL was 0.01 ppm; therefore, we have to conduct research on preparing safety standards for mushrooms, including L. edodes.

Safety on Hazardous Substances of Soeumin Kwakhyangjeonggi-san (소음인(少陰人) 곽향정기산(藿香正氣散)의 위해물질에 대한 안전성 연구)

  • Seo, Chang-Seob;Kim, Jung-Hoon;Huang, Dae-Sun;Shin, Hyeun-Kyoo
    • Journal of Sasang Constitutional Medicine
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    • v.22 no.3
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    • pp.132-140
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    • 2010
  • 1. Objective: To compare the contents and transfer rate of hazardous substances in crude, washing solution, crude after washing, decoction and remnant after boiling. 2. Methods: The heavy metal contents of each step were measured by inductively coupled plasma mass spectrometer (ICP-MS) and mercury analyzer (MA-2). In order to analyze pesticides in each sample 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. In addition, the contents of sulfur dioxide (SO2) were performed by Monier-Williams distillation method. 3. Results: 1) Contents (mg/kg) of heavy metals in decoction of all herbal medicine prescriptions were not detected. 2) Transfer rates (%) of heavy metals from crude to remnant were As (83.3%), Cd (100.0%), Pb (182.6%) and Hg (100.0%). 3) Contents (mg/kg) of residual pesticides were not detected. 4) Transfer rate (%) of sulfur dioxide (SO2) from crude to remnant was 44.2%. 4. Conclusion: Our results showed that boiled herbal medicine prescriptions which we take is safe from the hazardous substances.

Multiresidue Analysis of 240 Pesticides in Apple and Lettuce by QuEChERS Sample Preparation and HPLC-MS/MS Analysis (QuEChERS 전처리법과 HPLC-MS/MS 기기분석을 이용한 사과와 상추 중 240종 농약의 동시분석)

  • Kwon, Hye-Young;Kim, Chan-Sub;Park, Byung-Jun;Jin, Yong-Duk;Son, Kyung-Ae;Hong, Su-Myeong;Lee, Je-Bong;Im, Geon-Jae
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.417-433
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    • 2011
  • The study tested QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation and HPLC-MS/ MS analysis for measurement of pesticide residues in fruit and vegetable. 240 kinds of pesticides spiked at three levels of 90, 45, 9 ng/g in lettuce and apple. For QuEChERS sample preparation, graphitized carbon black (GCB) was used for only lettuce in dispersive-SPE as absorbent. Matrix-matched standard calibration was used for quantitative analysis of HPLC-MS/MS. 218 pesticides (91%) in apple and 207 pesticides (86%) in lettuce showed recoveries in the range of 70~120% with $RSD{\leq}20%$. The lowest calibrated level (LCL) were 4.5 ng/g for 192 pesticides, 9 ng/g for 42 pesticides, 45 ng/g for 3 pesticides and 3 pesticides were not detected at all concentration levels. The results showed that the QuEChERS sample preparation and HPLC-MS/MS analysis can be applied to multi-residue analysis of pesticides in vegetables and fruits.