• Title/Summary/Keyword: DAD analysis

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A Study on External.Internal Morphology and Pattern Analysis of Atractylodes Rhizomes (출류(朮類) 한약재의 외.내부형태와 이화학패턴 연구)

  • Kim, Jung-Hoon;Lee, Guem-San;Choil, Goya;Hwang, Sung-Yeoun;Kim, Hong-Jun;Jeong, Seung-Il;Ju, Young-Sung
    • The Korea Journal of Herbology
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    • v.24 no.2
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    • pp.77-85
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    • 2009
  • Objectives : To determine the discriminative criteria for Atractylodes rhizomes, the experiment of externalinternal characteristics and physicochemical pattern analysis were performed. Methods : External characteristics was observed using stereoscope. The sectioned materials which were covered with parffin were stained by Ju's method. Physicochemical patterns were analyzed using HPLC/DAD. Results : 1. External shape of original plant : Atractylodes maaocephala and A. japonica had relatively long petioles and 3-5 parted leaves. A. macrocephala had big purple flowers whereas A. japonica had relatively small white flowers and pinnate bracts. A. lancea had sessile leaves and white flowers, and the end parts of degenerated stamens were bent. 2. External shape of herbal medicine: A. macrocephala which was fist-shaped rhizome had pa-pillate processes and the cross section was light gray and sulcate. A. japonica and A. lancea were connected-beady or tubercular rhizomes, and the cross sections were both yellow-colored white. However, the cross section of A. japonica was fibrous, the width of cortex was narro-wer than that of stele, and radial shape in cortex was rare, whereas the width of cortex in A. lancea was similar to that of stele in size, and radial shape in cortex was obvious. 3. Internal shape of herbal medicine: A. macrocephala and A. lancea did not have lignified fascicles in cortex. However, the vascular bundles and vessels of A. macrocephala were wedge shaped and radial arrangement, and vascular bundles were densely populated in stele whereas those of A. lancea were repeatedly arranged and thinly extended to cortex. A. japonica had lignified fascicles in cortex and the width of vascular bundles was conspicuously thick with narrow intervals. 4. Physicochemical pattern analysis : A. macrocephala and A. lancea contained atractylenolide I and atractylenolide Ill whereas A. japonica contained atractylenolide I, atractylenolide Ill. diacetyl-atractylodiol, compound-4, compound-5. The three species of Atractylodes rhizomes showed different chromatogram patterns. Conclusions : The results could be used as discriminative criteria for Atractylodes rhizomes and as fundamental materials to researches of further pattern analysis and biological reaction.

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%.

Establishment of Pre-Harvest Residue Limit (PHRL) of Fungicides Azoxystrobin and Difenoconazole on Prunus mume fruits (매실 중 살균제 azoxystrobin과 difenoconazole의 생산단계 잔류허용기준 설정)

  • Lee, Dong Yeol;Kim, Yeong Jin;Park, Min Ho;Lee, Seung Hwa;Kim, Sang Gon;Kang, Nam Jun;Kang, Kyu Young
    • The Korean Journal of Pesticide Science
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    • v.17 no.4
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    • pp.307-313
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    • 2013
  • This study was carried out to investigate the residual characteristics of fungicide azoxystrobin and difenoconazole in Prunus mume fruits, and establish pre-harvest residue limits (PHRL) based on dissipation and biological half-lives of fungicide residues. The fungicides were sprayed onto the crop at recommended dosage once and 3 times in 7 days interval, respectively. The samples were harvested at 0, 1, 2, 4, 6, 8, 10, 12 and 14 days after treatment. These residual pesticides were extracted with QuEChERS method, clean-up with $NH_2$ SPE cartridge, and residues were analyzed by HPLC/DAD and GLC/ECD, respectively. Method quantitative limits (MQL) of azoxystrobin were 0.03 mg $kg^{-1}$ and of difenoconazole were 0.006 mg $kg^{-1}$. Average recovery were $93.2{\pm}2.49%$, $85.5{\pm}1.97%$ for azoxystrobin at fortification levels at 0.3 and 1.5 mg $kg^{-1}$, and $100.8{\pm}6.74%$, $87.6{\pm}9.92%$ for difenoconazole at fortification levels at 0.06 and 0.3 mg $kg^{-1}$, respectively. The biological half-lives of azoxystrobin were 5.9 and 5.2 days at recommended dosage once and 3 times in 7 days interval, respectively. The biological half-lives of difenoconazole were 9.3 and 8.0 days at recommended dosage once and 3 times in 7 days interval, respectively. The PHRL of azoxystrobin and difenoconazole were recommended as 5.32 and 1.64 mg $kg^{-1}$ for 10 days before harvest, respectively.

Estimation of the Moisture Maximizing Rate based on the Moisture Inflow Direction : A Case Study of Typhoon Rusa in Gangneung Region (수분유입방향을 고려한 강릉지역 태풍 루사의 수분최대화비 산정)

  • Kim, Moon-Hyun;Jung, Il-Won;Im, Eun-Soon;Kwon, Won-Tae
    • Journal of Korea Water Resources Association
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    • v.40 no.9
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    • pp.697-707
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    • 2007
  • In this study, we estimated the PMP(Probable Maximum Precipitation) and its transition in case of the typhoon Rusa which happened the biggest damage of all typhoons in the Korea. Specially, we analysed the moisture maximizing rate under the consideration of meteorological condition based on the orographic property when it hits in Gangneung region. The PMP is calculated by the rate of the maximum persisting 12 hours 1000 hPa dew points and representative persisting 12 hours 1000 hPa dew point. The former is influenced by the moisture inflow regions. These regions are determined by the surface wind direction, 850 hPa moisture flux and streamline, which are the critically different aspects compared to that of previous study. The latter is calculated using statistics program (FARD2002) provided by NIDP(National Institute for Disaster Prevention). In this program, the dew point is calculated by reappearance period 50-year frequency analysis from 5% of the level of significant when probability distribution type is applied extreme type I (Gumbel distribution) and parameter estimation method is used the Moment method. So this study indicated for small basin$(3.76km^2)$ the difference the PMP through new method and through existing result of established storm transposition and DAD(Depth-Area-Duration). Consequently, the moisture maximizing rate is calculated in the moisture inflow regions determined by meteorological fields is higher $0.20{\sim}0.40$ range than that of previous study. And the precipitation is increased $16{\sim}31%$ when this rate is applied for calculation.

Evaluation of Antioxidant, Cytoprotective and Antimicrobial Properties of Polygoni multiflori Radix Extract, Fractions and Its Major Constituent (하수오 추출물, 분획물 및 주성분의 항산화, 세포 보호 및 항균 활성에 관한 평가)

  • Shin, Hyuk Soo;Kim, Minwoo;Song, Jerry;Lee, Junseok;Ha, Yoonjeong;Jeon, Young Hee;Kim, Ji Woong;Lee, Yun Ju;Park, Soo Nam
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.44 no.4
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    • pp.407-417
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    • 2018
  • In this study, the antioxidant, cytoprotective and antimicrobial activities of 50% ethanol extract of Polygoni multiflori Radix (PMR) and its ethyl acetate fraction were evaluated to confirm the applicability as a functional ingredient. The activities of the major constituent of PMR were verified and 2, 3, 5, 4′-tetrahydroxystilbene 2-O-${\beta}$-D-glucoside (THSG) was confirmed to be the main component of extract and fraction using HPLC-DAD, LC-EIS-MS analysis. The phenolic and THSG contents of the ethyl acetate fraction were 11.1- and 3.0-folds higher than those of the ethanol extract, respectively. As a result of the DPPH assay and that of luminol dependent chemiluminescence assay in $Fe^{3+}$-EDTA/H2O2 system. the ethylacetate fraction was superior to the ethanol extract in free radical and ROS scavenging activities. Especially, the ethyl acetate fraction and THSG exhibited the similar scavenging activity like L-ascorbic acid in ROS scavenging activity. The ethyl acetate fraction perceived the most potent cytoprotective effect against oxidative damage of erythrocytes induced by photosensitization reaction, followed by the ethanol fraction, THSG and that of (+)-${\alpha}$-tocopherol, which was used as a positive control. Antimicrobial activities were evaluated by disc diffusion and broth microdilution assay against S. aureus, E. coli, P. aeruginosa and C. albicans. In particular, the antibacterial activity of the extract and fraction against S. aureus was superior to that of methyl paraben. Taken together, our results suggest that PMR could be used as a natural ingredient for antioxidant, cytoprotective and antimicrobial activities.

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.

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 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.

The Effects of High Temperature High Pressure Steam Sterilization on Woohwangchungsimwon (고온고압증기멸균이 우황청심원에 미치는 영향)

  • Cho, Chang-Young;Lee, In-Hee;Lee, Jae-Woong;Kim, Eun-Jee;Lee, Jin-Ho;Kim, Min-Jeong
    • Journal of Korean Medicine Rehabilitation
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    • v.25 no.1
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    • pp.45-52
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    • 2015
  • Objectives To check marker content for appropriate quality control of Woohwangchungsimwon sterilized to ensure microbiological safety and to observe antioxidant activity for any changes in efficacy. Methods To measure any effects of sterilization on the effective compounds, 8 ingredients of Woohwangchungsimwon were screened for any changes in marker content using HPLC-DAD. Using the colorimetric method on the microplate reader any changes in total phenolic compound and flavonoid levels were observed. Antioxidant activity was measured using the DPPH, ABTS, and FRAP. Results Of the ingredients of Woohwangchungsimwon, 8 were subject to quantitative analysis before and after sterilization. 21.6 mg and 1.93 mg of Glycyrrhizin was found in Glycyrrhiza uralensis Fischer pre and post sterilization, respectively. Decursin found in Angelica gigas Nakai increased from 0.16 mg to 0.29 mg after sterilization. Bilirubin found in Gallstone of Bostaurusvar. domesticus increased from 0.24 mg to 0.33 mg. Cinnamic acid found in Cinnamomum cassia Blume increased from 0.02 mg to 0.05 mg. Ginsenoside Rb1 found in Panax ginseng C. A. Meyer decreased from 0.02 mg to 0.14 mg. Paeoniflorin found in Paeonia lactiflora Pallas increased from 1.05 mg to 1.13 mg. Amygdalin found in Armeniacae Amarum Semen increased from 2.68 mg to 2.83 mg. L-muscone found in Musk increased from 0.63 mg to 0.76 mg. As for total phenolic compound and total flavonoid content, there was a 1.22 and 4.15-fold increase. DPPH and ABTS increased by 20.45% and 20.69%, respectively. FRAP activity was 2.78 times more active post stabilization. Conclusions This study confirmed that high temperature high pressure steam sterilization, a method used to ensure microbiological safety of Woohwangchungsimwon, does not affect marker content; in other words, does not affect quality of the Woohwangchungsimwon. It could also be seen that total phenolic compound and flavonoid content increased after sterilization. An antioxidant activity test showed that there was significantly increased activity of antioxidants.