• Title/Summary/Keyword: HPLC-ECD

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Meliasendanins E-J, Nor-neolignan Constituents from Melia toosendan and their Anti-inflammatory Activity

  • Jin Woo Lee
    • Natural Product Sciences
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    • v.29 no.1
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    • pp.17-23
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    • 2023
  • A phytochemical investigation of the fruits extract of Melia toosendan afforded the isolation of two new nor-neolignans, meliasendanins E (1) and F (2), as well as twelve known compounds (3 - 14) using various separation technique such as Diaion HP20, silica, RP-18 gel column chromatography and semi-preparative HPLC. Their chemical structures were elucidated by extensive NMR spectroscopic data including 2D-NMR, and HR-ESI-MS as well as ECD data. Among the twelve known compounds, the absolute structures of 3 - 6 were determined first, and given the trivial names as meliasendanins G-J (3 - 6). Based on the evaluation of anti-inflammatory activity, compounds 7 - 8 exhibited inhibitory effects on LPS-induced nitric oxide production in RAW 264.7 macrophages with IC50 values of 34.6 and 39.5 µM, respectively.

Monitoring of Pesticide Residues in Commercial Environment-friendly Stalk and Stem Vegetables and Leafy Vegetables and Risk Assessment (유통 친환경 엽채류와 엽경채류 중 잔류농약 실태조사 및 안전성 평가)

  • Lee, Jae-Yun;Noh, Hyun-Ho;Lee, Kwang-Hun;Park, So-Hyun;Kyung, Kee-Sung
    • 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.

Residual Characteristics of Insecticides Used for Oriental Tobacco Budworm Control of Paprika (파프리카 재배기간 중 담배나방 방제에 사용되는 살충제의 잔류특성)

  • Lee, Dong Yeol;Kim, Yeong Jin;Kim, Sang Gon;Kang, Kyu Young
    • Korean Journal of Environmental Agriculture
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    • v.32 no.1
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    • pp.84-93
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    • 2013
  • BACKGROUND: This study was carried out to investigate the residual characteristics of insecticides used for Oriental Tobacco Budworm control and to establish the recommended pre-harvest residue limit leading to contribution in safety of paprika production. METHODS AND RESULTS: The recommended Pre-Harvest Residue Limits (PHRLs) of insecticides during cultivation of paprika were calculated from residue analyses of insecticides in fruits 1, 3, 5, 7, 10, 12, 15, 18 and 21 days after treatment. Paprika samples were extracted with QuEChERS method and cleaned-up with amino propyl SPE cartridge and PSA, and insecticide residues were analyzed either by HPLC/DAD or GLC/ECD. The limits of detection were 0.01 mg/kg for 5 insecticides. Average recoveries were $81.3{\pm}1.62%$-$98.3{\pm}1.58%$ of 5 insecticides at fortification levels of 0.1 and 0.5 mg/kg. The biological half-lives of the insecticides were 8.5 days for bifenthrin, 11.8 days for chlorantraniliprole, 16.8 days for chlorfenapyr, 7.1 days for lamda-cyhalothrin and 31.3 days for methoxyfenozide at recommended dosage, respectively. CONCLUSION(S): The pre-harvest residue limits for 10 days before harvest were recommended 1.05 mg/kg, 1.41 mg/kg, 0.93 mg/kg, 2.06 mg/kg and 1.08 mg/kg as bifenthrin, chlorantraniliprole, chlorfenapyr, lamda-cyhalothrin and methoxyfenozide, respectively. This study can provide good practical measures to produce safe paprika fruit by prevention of products from exceeding of MRLs at pre-harvest stage.

Processing and Reduction Factors of Pesticide Residues in Chinese Matrimony Vine and Jujube by Drying (구기자와 대추 중 잔류농약의 건조에 따른 가공계수 및 감소계수)

  • Lee, Eun-Young;Noh, Hyun-Ho;Park, Young-Soon;Kang, Kyung-Won;Lee, Kwang-Hyen;Park, Hyo-Kyung;Kwon, Chan-Hyeok;Im, Moo-Hyeog;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
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    • v.13 no.3
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    • pp.159-164
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    • 2009
  • This study was carried out to elucidate changes in concentration of pesticide residues in Chinese matrimony vine and jujube during drying. Test pesticides, triadimefon and triforine for chinese matrimony vine and methoxyfenozide and thiacloprid for jujube, which are commonly used for the crops in Korea, were treated to the crops by spraying and dipping. The pesticide residues in both fresh and dried Chinese matrimony vine and jujube were analyzed by using a GLC-ECD and an HPLC-DAD. Processing factors of the pesticides in Chinese matrimony vine and jujube by drying ranged from 1.41 to 2.28 and from 1.50 to 4.20, respectively. And reduction factors of the pesticides in the crops ranged from 0.29 to 0.47 and from 0.68 to 0.98, respectively. These results indicate that concentrations of the pesticides in the test crops increased after drying, while amounts of pesticides in them were diminished by drying.

A survey on pesticide residues of imported fruits circulated in Gyeonggido (경기도내 유통 수입과실류의 잔류농약 실태조사)

  • Cho, Yun-Sik;Kang, Jeong-Bok;Kim, Yang-Hee;Jeong, Jin-A;Huh, Jeong-Weon;Lee, So-Hyun;Lim, Young-Sik;Bae, Ho-Jeong;Kang, Heung-Gyu;Lee, Jeong-Hee;Jung, Eun-Sook;Lee, Byoung-Hoon;Park, Yong-Bok;Lee, Jong-Bok
    • The Korean Journal of Pesticide Science
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    • v.16 no.3
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    • pp.195-201
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    • 2012
  • We tested for pesticide residues in 124 samples of 22 different items of imported fruits circulated in Gyeonggido. Total 218 pesticides were analyzed by multi-residue method using gas chromatography/nitrogen phosphorus detector-electron capture detector (GC/NPD-ECD), time of flight/mass spectrometer (TOF/MS), ultra performance liquid chromatography/photo diode array (UPLC/PDA), high performance liquid chromatography/fluorescence detector (HPLC/FLD) and mass spectrometer (LC/MS/MS). The pesticides were detected in 18 fruits samples, ranging 0.003~0.3 mg/kg and no samples had violative residue. The separation test to 14 sample pesticides detected was conducted to monitor the current status of pesticide residues according to the partial characteristic. The pesticides were detected in 14 peels ranging 0.03~1.5 mg/kg and 2 fleshes in less than detection limits. These results indicate that imported fruits are safe when the human takes normally but even the small amount of pesticides is harmful when the human takes it in a prolonged period. Therefore, the pesticide residual amounts of imported friuts should be constantly monitored for food safety.

Monitoring and Risk Assessment of Pesticide Residues in Commercial Environment Friendly Fruits and Fruiting Vegetables (유통 친환경 과실류와 과채류 중 농약잔류 실태조사 및 안전성 평가)

  • Lee, Jae Yun;Noh, Hyun Ho;Park, So Hyun;Lee, Kwang Hun;Park, Hyo Kyoung;Hong, Su Myeong;Kim, Doo Ho;Kyung, Kee Sung
    • 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.

Monitoring of Pesticide Residues and Risk Assessment for Fruit Vegetables and Root Vegetables of Environment-friendly Certified and General Agricultural Products (국내 유통 농산물 중 과채류와 근채류의 잔류농약 모니터링 및 위해성 평가)

  • Ahn, Ji-Woon;Jeon, Young-Hwan;Hwang, Jeong-In;Kim, Hyo-Young;Kim, Ji-Hwan;Chung, Duck-Hwa;Kim, Jang-Eok
    • Korean Journal of Environmental Agriculture
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    • v.31 no.2
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    • pp.164-169
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    • 2012
  • BACKGROUND: This study was conducted to monitor the residue of pesticides and to assess their risk in domestic agricultural products, such as fruit vegetables, tomatoes, oriental melons and root vegetables, garlic, potatoes and onions. METHODS AND RESULTS: 250 samples containing both general and environment-friendly certified agricultural products were collected from traditional markets and supermarkets in 6 cities. 132 pesticides except for herbicides were analysed using the multi-residue methods by GC/ECD, GC/NPD and HPLC/UVD. 17 kinds of pesticides were detected from 42 samples, which were 32 general, 1 organic, 4 pesticide-free and 5 low pesticide agricultural products. Among those, myclobutanil detected in 1 potato and procymidone detected in 10 oriental melons were unregistered pesticides for using in Korea. Fenbuconazole detected in 1 potato and phorate detected in 1 tomato were exceeded over the MRLs established by Korea Food and Drug Administration. CONCLUSION: Based on these results, a risk assesment was conducted using a percentage of acceptable daily intake(%ADI). %ADI ranged from 0.0064% to 4.6035%, and showed these values have no effect on human health.

Monitoring and risk assessment of pesticide in school foodservice products in seoul, Korea (서울지역 학교급식 식재료의 잔류농약 위해성 평가)

  • Seo, Young-Ho;Moon, Kwang-Deog
    • Food Science and Preservation
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    • v.21 no.1
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    • pp.69-74
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    • 2014
  • We tested for residual pesticide levels in school foodservice agricultural products in Seoul, Korea from 2010 to 2012. A total of 316 samples of 23 different types of agricultural products were analyzed via gas chromatography-nitrogen phosphate detector (GC-NPD), an electron capture detector (GC-${\mu}ECD$), a mass spectrometry detector (GC-MSD), and a high performance liquid chromatography-ultraviolet detector (HPLC-UV). We used multi-analysis methods to analyze 185 different pesticide types. Among the selected agricultural products, residual pesticides were detected in 26 samples (8.2%), of which 6 samples (1.9%) exceeded the Korea Maximum Residue limits (MRLs). We detected pesticide residue in more than 65% of the Chwinamul, while 6 among 9 analyzed samples contained pesticide residue, and 1 sample exceeded the Korea MRLs. Among the 185 kinds of pesticides that we have tested, 18 were detected, while 7 of them were detected more than twice. Data obtained were then used for estimating the potential health risks associated with the exposures to these pesticides. The most critical commodity is carbofuran in the perilla leaves, which has contributed 3.8% to the hazard index (HI). These results showed that the detected pesticides could not be considered as a serious public health problem. Nevertheless, constant supervision is recommended.

Monitoring of Endocrine Disruptor-suspected Pesticide Residues in Greenhouse Soils and Evaluation of Their Leachability to Groundwater (시설재배 토양 중 내분비계장애 추정농약의 잔류 모니터링 및 지하수 용탈 가능성)

  • Noh, Hyun-Ho;Lee, Kwang-Hun;Lee, Jae-Yun;Park, Hyo-Kyung;Lee, Eun-Young;Hong, Su-Myung;Park, Young-Soon;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.441-452
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    • 2011
  • This study was carried out to survey the residual characteristics of endocrine disruptor (ED)-suspected pesticides in greenhouse soils and assess their leachabilites to groundwater. Greenhouse soils were collected from 40 sites of greenhouse in 2008 in Korea. Sixteen ED-suspected pesticides which had been using in Korea, such as alachlor, benomyl, carbaryl, cypermethrin, 2,4-D, dicofol, endosulfan, fenvalerate, malathion, mancozeb, metribuzin, metiram, methomyl, parathion, trifluralin, and vinclozolin, in the soils, were analyzed by chromatographic methods using GLC-ECD and HPLC-DAD/FLD. Limits of detection (LODs) of the test pesticides ranged from 0.0004 to 0.005 mg/kg. Recoveries of the target pesticides from soil ranged from 72.69 to 115.28%. Four pesticides including cypermethrin were detected in the range of from 0.001 to 2.019 mg/kg, representing that their detection rate from greenhouse soils was 37.5%. The highest detection rate was observed from endosulfan which was detected from 16 site soils of the total samples, indicating that endosulfan is persistent in soil because of its very low mobility and high adsorption characteristics in soil. Based on the groundwater ubiquity scores (GUSs) of the pesticides detected from greenhouse soils, most of them have little possibilities of groundwater contamination except the fungicide vinclozolin with some leaching potential because of high water solubility and very low soil adsorption property.

A Study on the Safety of Residual Pesticides in Cereal Grains and Pulses Agricultural Products Excluding Rice (잡곡 농산물의 잔류농약 안전성 조사)

  • Han, Na-Eun;Kim, Jae-Gwan;Yun, Hee-Jeong;Kang, Min-Seong;Cho, Young-Seon;Song, Ji-Won;Kim, Byeong-Tae;Lee, Seong-Nam;Choi, Ok-Kyung
    • Journal of Food Hygiene and Safety
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    • v.37 no.1
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    • pp.1-8
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    • 2022
  • In this study, the pesticide residues in 106 commercial cereal grains were monitored from February to July 2021. For the investigation, 40 domestic and 66 imported products from large, small-to-medium sized offline and online distribution channels, were collected and analyzed by using the multiresidue method for 341 pesticides on GC/ECD, GC/NPD, GC/MSMS, UPLC/PDA, HPLC/FLD, LC/MSMS. Pesticides were detected in total of 8 samples (7.5%), of which one was from big box retailers, two from small and medium-sized distribution stores, and five from online shopping mall. Five (4.7%) samples were found to have pesticide residues greater than the maximum residue limits (MRLs). The detected pesticides in kidney beans (1 case), mung beans (6 cases), and sorghum (1 case), were MGK-264, chlorpyrifos, thiamethoxam, malathion, piperonyl butoxide, and pirimiphos-methyl. Specifically, an excessive amount of thiamethoxam was found from the imported mung bean (5 cases).