• Title/Summary/Keyword: HPLC/DAD

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Analysis of Methoxyfenozide and Bentazone in Plant with HPLC by pH-Adjusted Liquid-liquid Partition Cleanup (pH조절 분배추출에 의한 식물체 중 Methoxyfenozide와 Bentazone의 HPLC 분석)

  • Lo, Seog-Cho;Hwang, Cheol-Hwan;Yoo, Ki-Yong;Han, Seong-Soo
    • Korean Journal of Environmental Agriculture
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    • v.26 no.3
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    • pp.246-253
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    • 2007
  • This study was performed to enhance the cleanup efficiency of methoxyfenozide and bentazone by pH adjustment in the course of liquid-liquid partition and to develop an optimum analytical conditions using HPLC coupled with DAD for two matrices, brown rice and rice straw. Preparation procedure of brown rice sample was "extraction${\rightarrow}$coagulation${\rightarrow}$liquid-liquid partition$\rightarrow$-florisil C.C", and this procedure was samely applied to two compounds. In rice straw, preparation procedure of methoxyfenozide sample was "extraction$\rightarrow$-alkalization$\rightarrow$liquid-liquid extraction$\rightarrow$coagulation$\rightarrow$florisil C.C", and in the case of bentazone, "extraction$\rightarrow$alkalization$\rightarrow$liquid-liquid partition$\rightarrow$acidification$\rightarrow$liquid-liquid extraction$\rightarrow$florisil C.C". All these purified samples were redissolved in the mobile phases, acetonitile : 20 mM sodium acetate (75:25, v/v) for methoxyfenozide and acetonitrile : 75 mM sodium acetate, pH 6.0 (40:60, v/v) for bentazone. Recoveries of methoxyfenozide analysis in brown rice and rice straw were 83.5-97.4 and 86.4-97.3%, and detection limits were 0.02 and 0.04 mg/kg, respectively. Recoveries of bentazone in brown rice and rice straw were 86.8-101.9 and 88.3-94.5% and detection limits were 0.005 and 0.01 mg/kg, respectively. This methods seem to be usefully applied to the residue analysis of two compounds in the view of producing stable analytical condition and fair reproducibility.

Residue Dissipation Patterns of Neonicotinoid Acetamiprid and Thiamethoxam in Swiss Chard for the Harvest Periods under Greenhouse Conditions (시설재배 근대 중 Neonicotinoid계 살충제 Acetamiprid 및 Thiamethoxam의 생산단계 잔류특성)

  • Chang, Hee-Ra;You, Jung-Sun;Do, Jung-Ah
    • Korean Journal of Environmental Agriculture
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    • v.37 no.2
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    • pp.97-103
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    • 2018
  • BACKGROUND: Dissipation of acetamiprid and thiamethoxam in greenhouse grown chard samples was evaluated at 5 intervals including the pre-harvest interval after application. This study was conducted to determine the residue levels, the biological half-lives and dissipation rate of acetamiprid and thiamethoxam in chard under controlled conditions. METHODS AND RESULTS: Acetamiprid and thiamethoxam were applied in accordance with good agricultural practices for chard. Chard samples were collected at 0, 1, 2, 3, 5, 7, 10 and 14 days after application. Quantitaion was performed by HPLC-DAD system with C18 column. Limit of quantification (LOQ) of acetamiprid and thiamethoxam were both 0.02 mg/kg for chard. The recovery of acetamiprid and thiamethoxam were 77.8~107.5% and 94.3~108.6% at two concentration levels. The half-lives of pesticide dissipation in chard for two fields were 11.9 and 8.2 days for acetamiprid and 3.6 and 3.3 days for thiamethoxam respectively. The dissipation rate of acetamiprid and thiamethoxam were estimated according to the statistics method with a 95% confidence. CONCLUSION: Dissipation of acetamiprid and thiamethoxam in chard were determined under greenhouse. The concentration of acetamiprid and thiamethoxam in chards at 0 days after application were below specified by Korean MRL. Dissipation rate constant will be useful to set the pre-harvest residue limit for public health and consumer protection.

Usage Patterns of Feminine Hygiene Products and Preservative Contents in Feminine Cleansers in the Korean Market (국내 판매중인 여성청결제의 사용실태 및 함유 보존제 분석)

  • Kim, Wanseo;Youn, Youngin;Lee, Gowoon;Park, Na-Youn;Kho, Younglim;Choi, Kyungho
    • Journal of Environmental Health Sciences
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    • v.44 no.2
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    • pp.115-123
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    • 2018
  • Objectives: Preservatives, suspected to be endocrine disrupting chemicals, are widely used in feminine hygiene products for the prevention of deterioration. Information regarding the usage patterns of feminine hygiene products and the concentrations of preservatives in these products is limited. The present study was conducted to investigate the use of feminine cleansers among Korean women and quantify the concentration of preservatives in feminine cleansers. Methods: Approximately 500 women were recruited from the city of Busan in August 2017 and a questionnaire survey was conducted on the use of feminine cleansers. Several major feminine hygiene products (n=69) were identified and selected for analysis of 22 preservatives. Following appropriate preparation, the products were analyzed by HPLC/DAD. Results: Over 70% of the participating women used at least one feminine cleanser. Marital status and parity were associated with the frequency of use. Liquid was most frequently used form of feminine cleanser (66.6%). The greatest proportion of subjects answered that they use it 'one to two times per week' (36.5%). Among the 69 feminine cleansers, benzoic acid, sorbic acid, phenoxyethanol, and methyl paraben were detected at $144-4,428{\mu}g/g$, $195-1,470{\mu}g/g$, $269-4,237{\mu}g/g$, and $625-4,901{\mu}g/g$, respectively. BA was the most frequently detected (46.4%). Conclusions: In the present study, the characteristics of feminine cleanser use among Korean women were investigated. Based on an analysis of preservatives in the feminine hygiene products, one product was determined to exceed the maximum authorized concentration of MeP (0.4%). Our results will help refine exposure and risk assessment for toxic chemicals in feminine cleansers.

Establishment of Pre-Harvest Residue Limits (PHRLs) of Fungicide Fenarimol and Insecticide Flufenoxuron in Peaches during Cultivation Period (복숭아 재배기간 중 살균제 Fenarimol과 살충제 Flufenoxuron의 생산단계 잔류허용기준 설정)

  • Moon, Hye-Ree;Park, Jae-Hoon;Yoon, Ji-Yeong;Na, Eun-Shik;Lee, Kyu-Seung
    • Korean Journal of Environmental Agriculture
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    • v.32 no.2
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    • pp.136-141
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    • 2013
  • BACKGROUND: This study was performed to establishment the PHRLs of peach during cultivation period, and also to estimate biological half-lives for residues of fenarimol and flufenoxuron. METHODS AND RESULTS: The extracted samples of fenarimol were analyzed by GC-ECD and the flufenoxuron extracted samples were analyzed by HPLC-DAD. Recoveries of fenarimol at two fortification levels of 0.1 mg/kg, 0.5 mg/kg were $93.69{\pm}6.56$(%) and $94.45{\pm}1.60$ (%), respectively. And recoveries of flufenoxuron at two fortification levels of 0.1 mg/kg, 0.5 mg/kg were $106.73{\pm}5.90$(%) and $96.37{\pm}6.66$(%), respectively. CONCLUSION(S): The biological half-lives of fenarimol in single treatment and triple treatment were 3.5day and 3.8day. that of Flufenoxuron was also 7.1day and 4.9day, respectively. The PHRL of fenarimol were recommended as 1.5 mg/kg for 10day before harvest and the PHRL of flufenoxuron were recommended as 1.4 mg/kg for 10day before harvest.

Establishment of Pre-Harvest Residue Limits (PHRLs) of Insecticide Clothianidin and Fungicide Fluquinconazole on Peaches during Cultivation Period (복숭아의 재배기간 중 살충제 Clothianidin 및 살균제 Fluquinconazole의 생산단계 농약잔류허용기준의 설정)

  • Park, Jae-Hun;Lim, Jong-Sung;Yoon, Ji-Yeong;Moon, Hye-Ree;Han, Ye-Hoon;Lee, Yong-Jae;Lee, Kyu-Seung
    • Korean Journal of Environmental Agriculture
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    • v.31 no.3
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    • pp.271-276
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    • 2012
  • BACKGROUND: It is hard to control the agricultural products exceeding MRL (maximum residue limit) before forwarding. Therefore, NAQS (National Agricultural Products Quality Management Service, South Korea) established PHRL (pre-harvest residue limit) on agricultural products during their cultivation periods. This study was performed to set the PHRLs of peach during cultivation period, and also to estimate biological half-lives for residues of clothianidin and fluquinconazole. METHODS AND RESULTS: Two groups of peach were treated under Korean GAP (Good Agricultural Practices) with application time, single and triple treatments. Sample was collected over 14days (each after 0, 2, 4, 6, 8, 10, 12, 14 days. 8times), and clothianidin and fluquinconazole were analyzed by HPLC/DAD and GC/ECD, respectively. CONCLUSION: The biological half-life of clothianidin in single treatment and triple treatment was 5.2days and 7.0days. That of fluquinconazole was also 3.9days and 4.1days, respectively. The PHRL of peach on 10days before harvest was 1.4 mg/kg in clothianidin and 1.8 mg/kg in fluquinconazole.

Residue Dissipation Behavior of Bistrifluron and Cyenopyrafen in Peach for the Cultivation Periods under Field Conditions (노지재배 복숭아 중 Bistrifluron과 Cyenopyrafen의 생산단계 잔류특성에 따른 감소추이)

  • Hwang, Eun-Jin;Park, Jung-Eun;Kwon, Chan-Hyeok;Kim, Jin-Sook;Chang, Hee-Ra
    • Korean Journal of Environmental Agriculture
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    • v.37 no.1
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    • pp.41-48
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    • 2018
  • BACKGROUND: This study was performed to calculate the biological half-lives and regression coefficient of bistrifluron and cyenopyrafen dissipation in peach and to estimate the Pre-Harvest Residue Limits (PHRLs). METHODS AND RESULTS: The bistrifluron and cyenopyrafen were prepared on the basis of good agricultural practice for peach and treated with a single application. Peaches were harvested at 0, 1, 3, 5, 7, 10 and 14 days after application, prepared for analysis, and analyzed by HPLC-DAD. The limits of quantitation (LOQ) of bistifluron and cyenopyrafen were 0.02 mg/kg and 0.04 mg/kg, respectively. The recoveries of bistrifluron and cyenopyrafen were 99.5~108.7% and 88.4~98.9% at two different concentration levels. The biological half-lives of field I (Sejong) and field II (Pyeongtaek) were 6.1 and 7.0 days for bistifluron, and 6.3 and 7.0 days for cyenopyrafen, respectively. The 95% confidence intervals of dissipation rate constants of bistrifluron in peach were 0.0805~0.1457 and 0.0577~0.1417 for field I and field II, respectively, and those of cyenopyrafen were 0.0911~0.1278 and 0.0576~0.1417, respectively. CONCLUSION: Residue dissipation of bistrifluron and cyenopyrafen in peach were similar to that of correction to sample weight difference during the harvest periods. This study suggests that residue dissipation rate would be helpful to set the PHRLs that protect public health.

Quantitative Analysis of Atractylenolides I and III in Atractylodes japonica (백출의 Atractylenolide I과 Atractylenolide III의 함량분석)

  • Yun, Bo-Ra;Weon, Jin Bae;Lee, Bohyoung;Lee, Jiwoo;Eom, Min Rye;Ma, Choong Je
    • Korean Journal of Pharmacognosy
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    • v.44 no.1
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    • pp.53-59
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    • 2013
  • This study was conducted to determine the content of atractylenolides I and III in Atractylodes japonica. An established HPLC-DAD method was used to monitor contents of atractylenolides I and III in A. japonica obtained from Korea and China and compared with contents of A. macrocephala, A. chinensis, and A. lancea. Quantitative analysis of atractylenolides I and III was carried out on a Shiseido C18 column (S-5 ${\mu}m$, 4.6 mm I.D. ${\times}$ 250 mm) with gradient elution composed of acetonitile-water. The results show that the average content of atractylenolides I and III in A. japonica were 0.0954 and 0.1963%, respectively, and contents of A. lancea were higher than A. macrocephala, A. chinensis. In this study, we identified the differentiation of the quality of A. japonica from different species and collected locations and established content standard of atractylenolides I and III in A. japonica and this content standard was helpful to quality control of A. japonica.

Anthocyanin Profiling and Radical Scavenging Activity of Selected Pigmented Rice Varieties

  • Ali, Hiba A.;Cho, Il-Kyu;Kim, Sun-Ju;Kim, Se-Na;Kim, So-Young;Cho, Young-Sook;Baek, Hyung-Jin;Kim, Jung-Bong
    • Korean Journal of Environmental Agriculture
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    • v.30 no.2
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    • pp.111-117
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    • 2011
  • BACKGROUND: Anthocyanins have been recognized as health-enhancing substances due to their antioxidant activity, anti-inflammatory, anticancer, and hypoglycemic effects. The objective was to identify anthocyanins-rich rice grains for the development of functional foods and/or functional food colorants METHODS AND RESULTS: Rice grains of one black and three red-hulled rice varieties were extracted with acidified 80% aqueous methanol. The antioxidant activity of the methanolic extracts was screened on TLC plates and in an in vitro assay using DPPH (1, 1-diphenyl-2-picrylhydrazyl) as a free radical source. Red-hulled rice varieties exhibited higher antioxidant activity (88%, 1 mg/mL) than black rice (67%, 1 mg/mL). Among the red-hulled varieties tested, rice variety SSALBYEO54 (901452) was the most active (72%, 0.5 mg/mL). Rice extracted anthocyanin compounds were analyzed by HPLC-DAD-FLD and LC-MS/MS. Red-hulled varieties comprised cyanidin-3-glucoside in addition to ferulic acid esters, apigenin and kaempferol glycosides. CONCLUSION(s): Anthocyanins identified in the black rice variety were cyanidin-7-O-galactoside, cyanidin-3-Oglucoside, cyanidin-3'-O-glucoside, cyanidin-5-O-glucoside, cyanidin-3, 7-O-diglucoside, cyanidin-3, 5-O-diglucoside and peonidin-4'-O-glucoside. The results of this study show that the black rice (IT212512) and red-hulled rice variety SSALBYEO54 (901452) contain notable antioxidant activity for potential use in nutraceutical or functional food formulations.

Biological Activity and Inhibition of Non-Enzymatic Glycation by Methanolic Extract of Rosa davurica Pall. Roots

  • Hu, Weicheng;Han, Woong;Jiang, Yunyao;Wang, Myeong-Hyeon;Lee, Young-Mee
    • Preventive Nutrition and Food Science
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    • v.16 no.3
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    • pp.242-247
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    • 2011
  • The methanolic extract of Rosa davurica Pall. roots exhibited strong antioxidant activity in a 1,1-diphenyl-2-picryl-hydrazyl (DPPH) radical scavenging assay and was found to be a dose-dependent inhibitor of non-enzymatic formation of advanced glycation end products (AGEs), which are relevant to diabetes complications. HPLC-diode array detector (DAD) analysis of the R. davurica Pall. root extract led to the identification of four compounds: hydrocaffeic acid, catechin, epicatechin, and ellagic acid. Catechin was present in the largest amount and exhibited high antiglycation activity. A CYP3A4 assay was used to investigate potential interactions between drugs and the extract, and results suggest that the R. davurica Pall. root extract had moderate potential for interfering with drug metabolism. The R. davurica Pall. extract did not display anti-inflammatory activity on the level of that for tumor necrosis factor-${\alpha}$ (TNF-${\alpha}$) in a lipopolysaccharide (LPS)-stimulated macrophage assay; however, the extract did exhibit low to moderate immunostimulatory activity in a pro-inflammatory macrophage assay. Therefore, we conclude that R. davurica Pall. root is a promising anti-AGE agent with low to moderate risks of associated inflammation or drug interaction.

Comparison of Residue Patterns for Systemic and Non-systemic Pesticides in Strawberry (딸기 중 침투성 및 비침투성 농약에 따른 잔류특성 연구)

  • You, Jung-Sun;Gwak, Hye-Min;Chang, Hee-Ra
    • Korean Journal of Environmental Agriculture
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    • v.39 no.4
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    • pp.305-311
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    • 2020
  • BACKGROUND: The healthy food trend has encouraged the consumption of natural products, including berries. This trend is expected to increase the strawberry consumption. There has been a concern about the exposure of pesticides approved for use on strawberry. In this study, the dissipation patterns of systemic and non-systemic pesticides were evaluated in strawberry under plastic-covered greenhouse conditions. METHODS AND RESULTS: Cyflumetofen and dimethomorph were applied on strawberry in the critical GAP (Good Agricultural Practices). Strawberries were harvested at 0, 1, 2, 3, 5, 7 and 10 days after final application of the pesticides. The analyses of the residual pesticides were performed by HPLC-DAD with C18 column. The limits of quantitation (LOQ) of cyflumetofen and dimethomorph were 0.04 and 0.02 mg/kg, respectively. The recovery of cyflumetofen and dimethomorph were 88.1 ~ 103.3% and 79.0 ~ 110.2% for the spiked two levels (LOQ and 10LOQ), respectively. The biological half-lives of cyflumetofen and dimethomorph werer 7.5 and 8.9 days, respectively. The dissipation rates in strawberry were calculated by the statistics method at a 95% confidence level. The distribution showed that pesticides with low log Pow were indicated by the decreased dissipation rate and pesticides with similar log Pow and low solubility also showed the decreased dissipation rate. CONCLUSION: The residues of cyflumetofen and dimethomorph in strawberry at time 0 after the final application were below the established MRL in Korea. The dissipation behavior of systemic and non-systemic pesticides in strawberry is affected by their log Pow and water solubility values.