• Title/Summary/Keyword: HPLC/UVD

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High throughput approaches to predicting drug absorption potential using the immobilized artificial membrane phosphatidylcholine column and molar volume

  • Yoon, Chi-Ho;Shin, Beom-Soo;Chang, Hyun-Sook;Yoo, Sun-Dong
    • Proceedings of the PSK Conference
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    • pp.239.2-239
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    • 2003
  • The purpose of this study was to evaluate the predictability of the fraction of drug absorbed in humans using the immobilized artificial membrane phosphatidylcholine column (IAMPC) under optimized conditions in comparison with a conventional IAMPC method. Twenty commercial drugs, both acidic and basic in nature, were used in the study, Drugs were dissolved in acetonitrile:water (50:50, v/v) at a concentration of 100 mg/ml, and were injected on HPLC/UVD at a mobile phase (acetonitrile:DPBS = 10:90,v/v) with a flow rate of 0.5 ml/min equilibrated at 37$^{\circ}C$. (omitted)

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Determination of Dehydrocorydaline in the Corydalis Tuber Using HPLC-UVD (현호색의 품질 표준화 연구)

  • Kim, Jeong-Ah;Choi, Ji-Young;Kim, Dong-Chun;Lee, Hee-Sang;Lee, Seung-Ho
    • Korean Journal of Pharmacognosy
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    • v.39 no.4
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    • pp.305-309
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    • 2008
  • Dehydrocorydaline was isolated from the roots of Corydalis ternata (Papaveraceae) and identified by the comparison the $^1H-$ and $^{13}C$-NMR spectral data with those of authentic sample. The content of dehydrocorydaline was determined by the HPLC analysis based on extraction of ground plant material. Quantitative analysis of dehydrocorydaline in MeOH extract of C. ternata by HPLC showed $1.31{\pm}0.95%$ in 20 samples collected throughout regions of Korea.

Residual Pattern of Pesticide, Chlorfluazuron in Perilla Leaves Under Plastic House (들깻잎 재배 중 chlorfluazuron의 잔류량 변화 및 잔류분석법 시험)

  • Lee, Min-Ho;Kim, Seok-Ho;Park, Young-Guin;Jo, Gyeong-Yeon;Shin, Byung-Gon;Kim, Jong-Han;Kwon, Chan-Hyeok;Sohn, Jae-Keun;Kim, Jang-Eok
    • The Korean Journal of Pesticide Science
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    • v.11 no.2
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    • pp.106-116
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    • 2007
  • Pesticide, chlorfluazuron was subjected to determine the safety of terminal residues at the harvesting date of perilla leaves cultivated in plastic house. After the pesticide applied on a foliar spray in 2005 and 2006, leaf persistence of its residue was analysed for 10 days before leaf harvest. The degradation rate of chlorfluazuron in the leaf was 32.3 %(standard application), 43.6 %(double application) and 78.0 %(standard), 80.4 %(double) at second and tenth day, respectively, under analysis of GC/ECD in 2005. The degradation rate of chlorfluazuron in the leaf was 33.1 %(GC/ECD analyze), 34.0 %(HPLC/UVD analyze) and 77.9 %(GC/ECD), 78.4 %(HPLC/UVD) at second and tenth day, respectively, under the standard level of pesticide in 2006. The biological half-life of the chlorfluazuron residue was estimated by the regression equation calculated from daily dissipation of pesticide in the perilla leaves. The longest half-life of the chlorfluazuron residue in perilla leaves was 5.5 days. The maximum residual limit(MRL) for chlorfluazuron based on the longest half-life was estimated 2.0ppm at harvesting day, 2.5ppm at second day and 7.1ppm at tenth day before leaf harvesting of perilla.

Analysis of Pesticide Residues in Rice Straw for Livestock Feed (사료용 볏짚 중 잔류농약 분석)

  • Gil, Geun-Hwan;Kim, Jin-Bae;Kim, Chan-Sub;Son, Gyeong-Ae;Gwon, Hye-Yeong;Park, Jea-Eup;Lee, Kyu-Seung
    • The Korean Journal of Pesticide Science
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    • v.16 no.4
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    • pp.273-281
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    • 2012
  • This study was conducted for the establishment of the analytical method of pesticide residues in rice straw for 9 pesticides; etofenprox, tricyclazole, diazinon, edifenphos, propiconazole, carbaryl, carbofuran, 3-hydroxy carbofuran and 3-keto carbofuran and for the monitoring of these pesticides in rice straw for livestock feed in Korea. These pesticides were classified into 4 groups according to analytical instrument condition. Group 1 (HPLC-UVD1) included tricyclazole and etofenprox while group 2 (HPLC-UVD2) included propiconazole and edifenphos. Group 3 (HPLC-FLD) included carbaryl, carbofuran, 3-hydroxy carbofuran and 3-keto carbofuran. Group 4 (GC-NPD) included Diazinon. The dried rice straw samples were extracted with acetone and purified by liquid-liquid partition and solid phase extraction (SPE): Combination of Florisil SPE and amino-propyl SPE was used for group 1 and group 2, amino-propyl SPE for group 3, and Florisil SPE was for group 4. Recovery was in the ranged 70~110% and the limits of quantitation (LOQ) were lower than the half of maximum residue limits. Therefore this method was proved to be efficient for monitoring of these pesticides residue in rice straw. A total of 18 rice straw samples from 6 provinces in Korea in 2010 were analyzed using established method and, only 3-keto carbofuran was detected in one sample at concentration of 0.04 mg/kg.

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.

Residue Patterns and Biological Half-lives of Pyridalyl and Fluopicolide in Watermelon (수박 중 및 Pyridalyl 및 Fluopicolide의 잔류 특성 및 생물학적 반감기 산출)

  • Park, Ji-Su;Yang, Seung-Hyun;Choi, Hoon
    • Korean Journal of Environmental Agriculture
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    • v.36 no.1
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    • pp.50-56
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    • 2017
  • BACKGROUND: The present study was carried out to identify the residue patterns of insecticide pyridalyl and fungicide fluopicolide in watermelon and calculate the biological half-lives for establishing the pre-harvest residue limits (PHRLs). METHODSANDRESULTS:The watermelon samples for residue analysis were harvested 7 times during 0~10 days (Field 1) and 0~20 days (Field 2) after treatment of pesticides on watermelon in two different fields at the recommended dose, respectively. The residue analysis was conducted with HPLC/UVD. The method limit of quantitation (MLOQ) were set at 0.05 and 0.02 mg/kg, respectively, and overall mean recoveries were 81.2~90.5% for pyridalyl and fluopicolide. The residues in sample were stable for 43~47 days. The initial residue amount in field 1 and 2 were 0.12~0.16 mg/kg for pyridalyl and 0.23~0.24 mg/kg for fluopicolide, which were below maximum residue limit (MRL). The biological half-lives in field 1 and 2 were 26.9 and 17.9 days for pyridalyl and 16.6 and 94.2 days for fluopicolide, respectively. CONCLUSION: The PHRL for watermelon were estimated as 0.21 and 1.03 mg/kg for pyridalyl and flopicolide at 10 days before harvesting. The residue patterns of pyridalyl and fluopicolide were characterized by a very slow decrease of residue levels in watermelon.

Pharmacokinetics of amoxicillin after intramuscular injection at different temperatures to cultured olive flounder, Paralichthys olivaceus (Amoxicillin의 근육투여에 따른 수온별 넙치 체내 약동학적 특성)

  • Kim, Ji-Soo;Lee, Ji-Hoon;Lee, Soo-Jin;Park, Kwan-Ha
    • Journal of fish pathology
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    • v.28 no.1
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    • pp.43-51
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    • 2015
  • The pharmacokinetic properties and residue levels of amoxicillin (AMOX) were studied after intramuscular injection to cultured olive flounders ($100{\pm}50g$), Paralichthys olivaceus. For pharmacokinetic studies, AMOX of 20 to 80 mg/kg body weight was administered at $17{\pm}2^{\circ}C$ or $22{\pm}2^{\circ}C$ and AMOX concentrations were determined in plasma, the liver, and the kidney by HPLC-UVD. Plasma samples were assessed at 0.25, 0.5, 1, 3, 6, 12, 24, 48, 72, 96, 168 hours post-dose, whereas liver and kidney concentrations were measured at 0.25 to 48 hours post-dose. The kinetic profiles of AMOX were analyzed by fitting to a 2-compartmental model with PKSolver program. The following parameters were obtained for a single dosage of 20, 40 and 80 mg/kg of body weight at $22^{\circ}C$ and 20 and 40 mg/kg of body weight at $17^{\circ}C$ in plasma, liver and kidney, respectively: $C_{max}$ (the peak concentration)= $27.23-257.36{\mu}g/m{\ell}$, $5.49-41.65{\mu}g/g$, $16.75-129.31{\mu}g/g$; $t_{max}$ (the time for peak concentration)= 0.05-0.91, 1.36-3.28, 1.95-4.49 h. For residue studies, AMOX of 40 and 400mg/kg was administered, and muscle samples were taken at 2, 5, 7, 14 and 21 days post-dose. The residueof AMOX in the muscle were found under the MRLs (maximum residue levels) within 7 days for the two doses.

Validation and Uncertainty Evaluation of an Optimized Analytical Method Using HPLC Applied to Canthaxanthin, a Food Colorant (식품 색소 Canthaxanthin의 HPLC 최적 분석법 확인 및 타당성과 측정불확도 평가)

  • Suh, Hee-Jae;Kim, Kyung-Su;Hong, Mi-Na;Lee, Chan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.3
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    • pp.342-351
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    • 2016
  • This study was carried out to develop an optimized analytical method using high-performance liquid chromatography (HPLC) applied to canthaxanthin, which is not yet designated as a food colorant in Korea, as well as to perform validation and uncertainty evaluation of this method. Official methods of AOAC, UK, and Japan with HPLC-UV detection were evaluated for the analysis of canthaxanthin by comparison of linearity, resolution, selectivity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision, recovery, inter-laboratory tests, and uncertainty measurement. The calibration curves showed high linearity with an $R_2$ value of over 0.999 for canthaxanthin standard solutions in all three official methods. The official method of Japan exhibited the best results in terms of resolution and selectivity, including the lowest LOD and LOQ. The average coefficients of variation were calculated as less than five of three institutes with a precision value less than 1, accuracy near 100%, and recovery ratio between $100{\pm}10%$. The expanded uncertainty for canthaxanthin was estimated to be $39.5{\pm}5.29mg/kg$ (95% confidence level, k=2), and the uncertainty of measurement was 13.4%. In this study, official methods of canthaxanthin were compared and the validities verified. The results will be further applied to establish an authorized analytical method for canthaxanthin in Korea.

Monitoring of Pesticide Residues in Special Products (지역특산품 중 잔류농약 실태조사)

  • Kim, Mi-Ra;Na, Mi-Ae;Jung, Woo-Young;Kim, Chang-Soo;Sun, Nam-Kyu;Seo, Eun-Chae;Lee, Eun-Mi;Park, You-Gyoung;Byun, Jung-Ah;Eom, Joon-Ho;Jung, Rae-Seok;Lee, Jin-Ha
    • The Korean Journal of Pesticide Science
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    • v.12 no.4
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    • pp.323-334
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    • 2008
  • This experiment was carried out to analyze for pesticide residues in 17 different types of the special of geographical indication. We purchased 3 cereal grains, nuts and seeds, 3 fruits, 8 vegetables, mushrooms and other plants (Korean medicines) mainly at the agricultural cooperative's joints markets. Total 209 pesticides including multi-analysed pesticides (204) and single-analysed pesticides (5 ; acephate, methamidophos, monocrotophos, omethoate, vamidothion) were analysed with a GC/MS/MS, an HPLC/UVD (PDA) and a GC/FPD. No. 83 method and single-analysed method (Screening of multi-pesticide residue in the special products of geographical indication) of Korea Food Code was selected for validation in recovery and interferences of matrice. The results were as follows: among the selected 17 the special products, the residual pesticides were detected in 8 types of the special products (40 in 302 samples, detection ratio; 13.2%). All of the samples were not detected over MRLs, but tebuconazole, procymidone and isoprothioran were detected with considerable high frequency. These results could be used as KFDA official methods for the analysis of pesticide residues in foods and reference data will be provided to the related institutions.

Determination of Pyribencarb and Its Metabolite KIE-9749 in Agricultural Commodities by High-Performance Liquid Chromatography (액체크로마토그래피를 이용한 농산물중 pyribencarb와 대사물 KIE-9749의 잔류 분석법)

  • Kwon, Hyeyoung;Hong, Su-Myeong;Kim, Taek-Kyum;Kim, Hyung-Jin;Moon, Byeong-Chul;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
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    • v.20 no.3
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    • pp.236-246
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    • 2016
  • The aim of this study was to develop an analytical method for the determination of pyribencarb and its metabolite KIE-9749 in agricultural commodities. The experiment was performed with a range of concentrations $0.05{\sim}2.5{\mu}g/g$ in apple, green pepper, potato, hulled rice, soybean, pear, peach, grape and cucumber. Each samples were extracted with acetone and cleaned by dichloromethane/saline water partition and purified with Florisil solid phase extraction (SPE) cartridge and aminopropyl SPE cartridge. Pyribencarb and KIE-9749 were separated and quantified by HPLC/UVD at 265nm using acetonitrile and water as mobile phase. The recoveries of pyribencarb and KIE-9749 were within 78.3~108.4% and 73.9~113.7% with RSD below 12.2% and 15.0%, respectively. The limits of quantification (LOQ) were both $0.05{\mu}g/g$. LC/ESI-MS/MS was optimized for confirmation of residue identity.