• Title/Summary/Keyword: DAD

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Risk Assessment of the Exposure to Rotenone in Lettuce and Cucumber (상추, 오이 섭취에 따른 rotenone의 위해성 평가)

  • Choi, Ji Hee;Woo, Hye-Im;Jeong, Ye-Ji;Noh, Hyun Ho;Kyung, Kee Sung;Kim, Doo-Ho;Paik, Min-Kyung;Om, Ae Son
    • The Korean Journal of Pesticide Science
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    • v.17 no.4
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    • pp.302-306
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    • 2013
  • We report the dietary exposure to rotenone in the Korean population and children (1-18) through consumption of lettuce and cucumber. To obtain the residue data, we analyzed using the GC-NPD and HPLC-DAD method. Rotenone residues in samples were as follows; lettuce 0.16-1.15, cucumber < 0.001-0.006. The average dietary intake was determined using result from the 2009 Korea National Health and Nutrition Examination Survey Data. The risk index (RI) was calculated using rotenone residues and dietary intakes. The lettuce and cucumber showed the highest at 18.41%, 0.00, respectively. RI fell below 100 of %RfD showing no risks in these vegetables. Therefore, the risk assessment on the detected rotenone was evaluated as safe level.

Establishment of an Analytical Method for Azorubine, an Undesignated Food Colorant in Korea

  • Kim, Min-ji;Park, Ju-hee;Suh, Hee-Jae;Lee, Chan
    • Journal of Food Hygiene and Safety
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    • v.31 no.5
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    • pp.311-318
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    • 2016
  • Azorubine is a synthetic tar color containing azo-bond in the molecular structure. This food colorant has been allowed to be used for beverages, cheese and dried fruits in the European Union and for some food in Australia. Even though it is applicable as a food color in many countries, this compound has not been permitted in Korea so far as a food additive. Thus, this study was performed to establish an analysis method for azorubine in Korea by comparison of three HPLC analysis methods for azorubine and other azo-compounds which are officially used in the European Food Safety Authority (EFSA, EU), the Food Standard Agency (FSA, England) and the National Institute of Food and Drug Safety Evaluation (NIFDS, Korea). The analysis method of the FSA for azorubine showed the best linearity ($r^2=0.999$), limit of detection (LOD, $0.07{\mu}g/mL$), limit of quantification (LOQ, $0.20{\mu}g/mL$), precision (0~0.5%) and accuracy (98.6~100.7%) among tested HPLC methods using a C-18 column and diode array detector (DAD) with ammonium acetate solution and acetonitrile as an eluent solution. Finally selected method of FSA was further verified by inter-day and intra-day experiments with linearity, LOD, LOQ, precision and accuracy. Recovery test showed the recover ratios of 97~103%, 95~101%, and 93~102% in beverages, breads/snacks and other foods, respectively. Inter-laboratory test represented the absolute value of z-score of less than 2 which means satisfactory levels in this test. Selected method of FSA showed reliable analytical results in application test using food samples collected in commercial markets in Europe.

Development of Analytical Method for Quality Control from New Herbal Medicine(HPL-4) (새로운 생약복합제제(HPL-4)의 품질관리를 위한 분석법 개발)

  • Kim, Se-Gun;Sharma, Dipak Kumar;Lamichhane, Ramakanta;Lee, Kyung-Hee;Han, Sang-Mi;Jung, Hyun-Ju
    • Korean Journal of Pharmacognosy
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    • v.45 no.4
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    • pp.338-345
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    • 2014
  • HPL-4 is a new herbal formulation developed for the treatment of osteoarthritis. In this study, we took HPL-4 to develop a method for simultaneous determination of nine marker compounds (protocatechuic acid, chlorogenic acid, liriodendrin, nodakenin, ${\beta}$-$\small{D}$-(3-O-sinapoyl)frucofuranosyl-${\alpha}$-$\small{D}$-(6-O-sinapoyl)glucopyranoside, quercitrin, 6-gingerol, decursin and decursinol angelate) present in the formulation. The analytes were separated by UPLC system consisting of diode array detector at 205 nm and RP-amide column, and solvent system of $ACN/0.1%H_3PO_4$. Analytical method was validated to evaluate its linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy. All standards showed good linearity ($R^2$ >0.99) in the rage of $0.25-400.0{\mu}g/mL$. The LOD and LOQ were within the range of 0.021-0.148 and $0.070-0.448{\mu}g/mL$, respectively. Intra- and inter-day precision was less than RSD 4.0% and the accuracy was range from 92.00-104.81% with RSD<4.2%. The results suggest that the developed UPLC method is precise, accurate and effective, and could be applied for quality control of HPL-4 formulation.

Residual Characteristics of Bistrifluron and Fluopicolide in Korean Cabbage for Establishing Pre-Harvest Residue Limit (생산단계 잔류허용기준 설정을 위한 엇갈이배추 중 bistrifluron과 fluopicolide의 잔류 특성 연구)

  • Lee, Dong Yeol;Jeong, Dong Kyu;Choi, Geun-Hyoung;Lee, Deuk-Yeong;Kang, Kyu Young;Kim, Jin Hyo
    • The Korean Journal of Pesticide Science
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    • v.19 no.4
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    • pp.361-369
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    • 2015
  • This study investigated residual characteristics of bistrifluron and fluopicolide in Korean cabbage, and suggested the pre-harvest residue limits (PHRLs) based on their dissipation patterns and biological half-lives. The pesticides were sprayed on Korean cabbage in two different region under greenhouse conditions at the recommended dose, respectively. The samples for residue analysis were harvested at 0 (2 hr), 1, 2, 4, 6, 8 and 10 days after treatment, and analyzed by HPLC after clean-up with Florisil SPE. The limit of quantification (LOQ) was $0.03mg\;kg^{-1}$ for bistrifluron and fluopicolide, and the recoveries ranged from 87.2-110.6% with below 5% of RSD. The biological half-lives of field I and field II were 3.9 and 4.2 days for bistrifluron and 4.9 and 4.2 days for fluopicolide, respectively. The PHRL of bistrifluron and fluopicolide were recommended as 3.83 and $3.23mg\;kg^{-1}$ for 10 days before harvest, respectively.

Establishment of Analytical Method for Pymetrozine Residues in Crops Using Liquid-Liquid Extraction(LLE) (액-액 분배법을 활용한 작물 중 pymetrozine의 잔류분석법 확립)

  • Yoon, Ji-Young;Moon, Hye-Ree;Park, Jae-Hun;Han, Ye-Hoon;Lee, Kyu-Seung
    • The Korean Journal of Pesticide Science
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    • v.17 no.2
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    • pp.107-116
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    • 2013
  • Polar pesticides like pymetrozine (log $P_{ow}$: -0.18) are known to be difficult to analyze. The analytical method of pymetrozine using hydromatrix included in the official method of KFDA was uncommon and provided ambiguous evidence to confirm both the identity and the quantity. Therefore, precise single residue analytical method was developed in representative crops for using liquid-liquid extraction (LLE). The pymetrozine residue was extracted with methanol from 11 representative crops which comprised apple, blueberry, broccoli, cabbage, cherry, crown daisy, hulled rice, Korean cabbage, potato, rice and watermelon. The extract was purified serially by liquid-liquid extraction (LLE) and silica solid phase extraction (SPE). For rice and hulled rice samples, n-hexane partition was additionally adopted to remove nonpolar interferences, mainly lipids. The residue levels were analyzed by HPLC with DAD, using $C_8$ column. LOQ (limit of quantitation) of pymetroizinie was 1 ng (S/N > 10) and MQL (method quantitation limit) was 0.01 mg/kg. Mean recoveries from 11 crop samples fortified at three levels (MQL, 10 ${\times}$ MQL and 50 ${\times}$ MQL) in triplicate were in the range of 83.1~98.5% with coefficients of variation (CV) of less than 10%, regardless of sample type, which satisfies the criteria of KFDA. The method established in this study could be applied to most of crops as an official and general method for analysis of pymetrozine residue.

Comparative Study on Antioxidant Capacities and Polyphenolic Contents of Commercially Available Cocoa-containing Products (유통되는 코코아함유 가공품의 항산화능과 폴리페놀 함량에 관한 연구)

  • Lee, Eun-Soon;Kum, Jin-Young;Hwang, Young-Ok;Tu, Ock-Ju;Jo, Han-Bin;Kim, Jung-Hun;Chae, Young-Zoo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.41 no.10
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    • pp.1356-1362
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    • 2012
  • UV-VIS spectrophotometric and high-performance liquid chromatographic (HPLC-DAD) methods were applied in order to identify and quantify the composition of polyphenols in commercial cocoa-containing products. Total polyphenolic contents of cocoa mix, choco-syrup, milk chocolate, and dark chocolate were evaluated using Folin-Ciocalteu's phenol reagent according to a UV-VIS spectrometric method. Antioxidant capacities of cocoa extracts by methanol were evaluated by 2,2'-azino-bis(3-ethyl benzothiazoline-6-sulfonic acid) (ABTS) assay and 2,2-diphenyl-1-picrylhydrazyl (DPPH) assay. The obtained results show that the polyphenolic contents and antioxidant capacities of cocoa products and chocolates depend on solid cocoa content. Among the tested cocoa products and chocolates, the most abundant phenolic compound was epicatechin.

Quantitative Analysis of Carotenoids in Carrot Cultivars Produced in Korea (국내산 당근 품종별 carotenoid 함량 분석)

  • Ha, Jeong-Lim;Bae, Jong-Sup;Park, Moon-Ki;Kim, Yong-Ung;Ha, Sun-Hwa;Bae, Jung-Myung;Back, Kyong-Whan;Lee, Cheol-Ho;Lee, Shin-Woo;Ahn, Mi-Jeong
    • Journal of Environmental Science International
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    • v.18 no.10
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    • pp.1135-1141
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    • 2009
  • Carrots (Daucus carota L.) are consumed as an important dietary source of provitamin A including $\beta$-carotene, $\alpha$-carotene and lutein. An HPLC method was applied to determine the content of the carotenoid composition in carrot cutivars cultivated in Korea. HPLC analyses were carried out with five carrot cultivars (Socheon-5-chon, Hongsim-5-chon, Myeongju-5-chon, Seonhongbom-5-chon and Betarich) sown at April, 2007 and six cultivars (Yeoreum-5-chon, Hanyeoreum-5-chon, Sinheukjeon-5-chon, Bibariheukjeon, Manina and Betarich) sown at August of the same year. In general, the former varieties are not used for the sowing at summer because of their bolting (growth of floral axis). The former and the latter carrots were harvested after 110 and 96 days from seeding, respectively, and the carotenoids were extracted with acetone after freeze-drying. The amount of $\alpha$-carotene ($117.7{\sim}205.3\;{\mu}g/g{\cdot}DW$) was similar to that of $\beta$-carotene ($113.1{\sim}189.6\;{\mu}g/g{\cdot}DW$) for the carrot cultivars sown at spring, while the content ($46.2{\sim}71.1\;{\mu}g/g{\cdot}DW$) was about a half of $\beta$-carotene content ($92.5{\sim}140.2\;{\mu}g/g{\cdot}DW$) for the latter cultivars. In addition, the average content of lutein ($25.2\;{\mu}g/g{\cdot}DW$) in the former cultivars was eight times higher than that in the latter cultivars ($3.1\;{\mu}g/g{\cdot}DW$). Among the spring cultivation types, Socheon-5-chon and Myeongju-5-chon showed higher amount of $\alpha$-carotene and $\beta$-carotene, while the higher amount was determined in Yeoreum-5-chon and Sinheukjeon-5-chon among the autumn cultivation types. Validation of the HPLC-DAD method showed good linearity ($r^2$ > 0.997) of the three compounds analyzed in a wide concentration range ($0.025{\sim}20\;{\mu}g/ml$). The R.S.D. values for intra-day and inter-day precision were less than 19.2% and the mean recovery of each compound was 85.4~104.7%.

Development of Method for Analysis of Four Sulfonylurea Pesticides, Rimsulfuron, Ethametsulfuron-methyl, Tribenuron-methyl, Chlorimuron-ethyl Residues by High-Performance Liquid Chromatography with Diode-Array Detection (HPLC/DAD를 이용한 림술푸론, 에타메트설푸론메틸, 트리베누론메칠, 클로리무론에칠 4종 성분의 잔류농약 분석법 개발)

  • Koo, Yun-Chang;Yang, Sung-Yong;Wang, Zeng;An, Eun-Mi;Heo, Kyoung;Kim, Hyeng-Kook;Shin, Han-Seung;Lee, Jin-Won;Lee, Kwang-Won
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.39 no.8
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    • pp.1231-1235
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    • 2010
  • The method for residue analysis of four sulfonylurea pesticides, rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl and chlorimuron-ethyl was examined and analyzed by HPLC with ODS column ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size) which was maintained at $35^{\circ}C$. Mobile phase consisted of solvent A (20 mM $KH_2PO_4$, pH 2.5) and solvent B (acetonitrile). Isocratic elution of the column with 45% solvent A and 55% solvent B at a flow rate of 1 mL/min resulted in retention times of 5.92, 6.54, 9.28, and 14.35 min for rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl, and chlorimuron-ethyl, respectively. All injection volumes were $20\;{\mu}L$. The limit of quantitation was 0.02, 0.01, 0.001, and 0.004 mg/kg for rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl, and chlorimuron-ethyl, respectively. Recovery rate test was performed with three farm products, rice, apple and soybean. Four sulfonylurea pesticides were spiked at concentrations of 0.05, 0.1 and 0.5 mg/kg. The recovery rates were ranged from 86.12% to 116.26% and the standard deviations of all experiments were within 10%.

Monitoring of Pesticide Residues in the Certificated Organic and Pesticide-free Cereals and Root Vegetables (유기 및 무농약 인증 곡류와 근채류 중 잔류농약 모니터링)

  • Lee, Jae Yun;Noh, Hyun Ho;Park, So Hyun;Jeong, Oh Seok;Kim, Seo Hong;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.401-405
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    • 2012
  • This study was carried out to investigate characteristics of the pesticide residues in environment friendly cereal grains and root vegetables. The samples, 747 the environment friendly agricultural products were collected from supermarkets and retail stores in eight major cities in May and August 2012. Residues of 245 pesticides in the samples collected were analyzed by multiresidue methods using GC and HPLC. No pesticide residues were detected in all the samples, representing the environment friendly cereal grains and root vegetables were produced according to the guideline for prohibition of use of pesticides during crop cultivation.

Future PMPs projection according to precipitation variation under RCP 8.5 climate change scenario (RCP 8.5 기후변화 시나리오의 강수량 변화에 따른 미래 PMPs의 전망)

  • Lee, Okjeong;Park, Myungwoo;Lee, Jeonghoon;Kim, Sangdan
    • Journal of Korea Water Resources Association
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    • v.49 no.2
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    • pp.107-119
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    • 2016
  • Since future climate scenarios indicate that extreme precipitation events will intensity, probable maximum precipitations (PMPs) without being taken climate change into account are very likely to be underestimated. In this study future PMPs in accordance with the variation of future rainfall are estimated. The hydro-meteorologic method is used to calculate PMPs. The orographic transposition factor is applied in place of the conventional terrain impact factor which has been used in previous PMPs estimation reports. Future DADs are indirectly obtained by using bias-correction and moving-averaged changing factor method based on daily precipitation projection under KMA RCM (HEDGEM3-RA) RCP 8.5 climate change scenario. As a result, future PMPs were found to increase and the spatially-averaged annual PMPs increase rate in 4-hour and $25km^2$ was projected to be 3 mm by 2045. In addition, the increased rate of future PMPs is growing increasingly in the future, but it is thought that the uncertainty of estimating PMPs caused by future precipitation projections is also increased in the distant future.