• Title/Summary/Keyword: polar column

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Domestic Research Trends on Fluorescent Dissolved Organic Matter in Marine Environment (해양 환경의 형광용존유기물에 관한 국내 연구 동향)

  • Kim, Jeonghyun
    • Ocean and Polar Research
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    • v.43 no.4
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    • pp.353-363
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    • 2021
  • Fluorescent dissolved organic matter (FDOM) is referred to organic matter which absorbs efficiently solar radiation energy and fluorescence in the water column. The component and molecular structure of marine organic matter can be changed depending on the various substances and origins of organic matter, and then the organic matter has unique fluorescent properties. As the cutting-edge analytical techniques of optical measurement continuously developing from last few decades, a study on FDOM has been applied as a biogeochemical tracer to quantify the organic matter concentration and to investigate the behaviors and origins of organic matter. Especially, the marine environment around the Korean Peninsula is an ideal research area to study FDOM because of various oceanographic characteristics and the origins of organic matter. This study describes the general properties of FDOM and introduces the cycling and behaviors of marine organic matter based on the domestic research studies.

Identification and HPLC Quantification of a Phytoecdysone and Three Phenolic Glycosides in Lamium takesimense Nakai

  • Nugroho, Agung;Park, Kyoung-Sik;Seo, Dong-Jin;Park, Hee-Juhn
    • Natural Product Sciences
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    • v.24 no.4
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    • pp.241-246
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    • 2018
  • The herbs of Lamium takesimense Nakai (Lamiaceae) is used to treat spasmodic and inflammatory disease. The four polar compounds, ecdysterone, isoacteoside, rutin and lamiuside C, were isolated and identified from the BuOH fraction of the L. takesimense MeOH extract. HPLC quantification was performed on a Capcell Pak C18 column ($5{\mu}m$, $4.6mm{\times}250mm$) with a gradient elution of $H_2O$ and 0.05% acetic acid in MeOH. The HPLC method was validated in terms of linearity, sensitivity, stability, precision, and accuracy. The quantitative level in plant material was determined as the following order: lamiuside C (4, 3.75 mg/g dry weight) > ecdysterone (1, 1.93 mg/g) > isoacteoside (2, 1.32 mg/g) > rutin (3, 0.97 mg/g).

Determination of Thiamine in Pharmaceutical Preparations by Reverse Phase Liquid Chromatography Without Use of Organic Solvent

  • Suh, Joon Hyuk;Kim, Junghyun;Jung, Juhee;Kim, Kyunghyun;Lee, Seul Gi;Cho, Hyun-Deok;Jung, Yura;Han, Sang Beom
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1745-1750
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    • 2013
  • A novel green aqueous mobile phase modified with room temperature ionic liquids (RTILs) was employed in the absence of volatile organic solvents or ion-pairing reagents to analyze thiamine, a very polar compound, by reverse phase high performance liquid chromatography (RP-HPLC). Due to its strongly hydrophilic nature, thiamine was eluted near the column dead time ($t_0$) using a mobile phase without adding RTILs or ion-pairing reagents, even if a 100% aqueous mobile phase, which has weak elution power under reverse phase conditions, was used. Thus, 1-ethyl-3-methyl-imidazolium hexafluorophosphate ([EMIM][$PF_6$]), which has the strongest chaotropic effect, was selected as a mobile phase additive to improve retention and avoid baseline disturbances at $t_0$. Various mobile phase parameters such as cation moiety, chaotropic anion moiety, pH and concentration of RTILs were optimized to determine thiamine at the proper retention time. Method validation was performed to assess linearity, intra- and inter-day accuracy and precision, recovery and repeatability; all results were found to be satisfactory. The developed method was also compared to the current official United States Pharmacopoeia (USP) and Korean Pharmacopoeia (KP) methods using an organic mobile phase containing an ionpairing reagent by means of evaluating various chromatographic parameters such as the capacity factor, theoretical plate number, peak asymmetry and tailing factor. The results indicated that the proposed method exhibited better efficiency of thiamine analysis than the official methods, and it was successfully applied to quantify thiamine in pharmaceutical preparations.

Seasonal Variation of Planktonic Foraminifera Assemblage in response to Seasonal Shift of Inter-Tropical Convergence Zone in the Northeastern Equatorial Pacific (적도수렴대의 위치변화에 따른 북동태평양 적도해역의 부유성 유공충 군집의 계절변동)

  • Lee, Yuri;Asahi, Hirofumi;Woo, Han Jun;Kim, Hyung Jeek;Lee, Seong-Joo;Khim, Boo-Keun
    • Ocean and Polar Research
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    • v.36 no.4
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    • pp.437-445
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    • 2014
  • A time-series sediment trap was operated at a water depth of 4950 m from July 2003 to May 2004 at KOMO station ($10^{\circ}30^{\prime}N$, $131^{\circ}20^{\prime}W$) in the northeastern equatorial Pacific, with the aim of understanding the temporal variation of planktonic foraminifera assemblages in response to the seasonal shift of Inter-Tropical Convergence Zone (ITCZ). A total of 22130 planktonic foraminifera specimens belonging to 30 species and 11 genera were identified, which shows a distinct seasonal variation with high values (125~288 specimens $m^{-2}day^{-1}$) in the winter to spring (December-May) and low values (16~23 specimens $m^{-2}day^{-1}$) in the fall (September-November). In addition, seasonal ecological differences of foraminifera assemblages are distinctly recognizable: omnivorous foraminifera occurred predominantly during the summer season, whereas herbivorous ones were dominant during the winter season. Such seasonal variations correspond to the seasonal shift of the ITCZ. Enhanced occurrence of herbivorous species during the winter-spring season seems a result of surface water mixing generated by the southward shift of the ITCZ. The increase in omnivorous species during the summer season may be due to the northward movement of the ITCZ caused by weakened wind speed, resulting in the intensification of water column stratification and nutrient-poor environment. A significant reduction of planktonic foraminifera specimens during the fall is attributed to heavy precipitation and reduction in light intensity.

Purification and Anticoagulant Activity of a Fucoidan from Korean Undaria pinnatifida Sporophyll

  • Kim , Woo-Jung;Kim, Sung-Min;Kim, Hyun-Guell;Oh, Hye-Rim;Lee, Kyung-Bok;Lee, Yoo-Kyung;Park, Yong-Il
    • ALGAE
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    • v.22 no.3
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    • pp.247-252
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    • 2007
  • Crude fucoidan was extracted from the sporophyll of Korean Undaria pinnatifida collected at a coastal area ofWando, Korea, mainly by dilute acid extraction, ethanol precipitation, CaCU Precipitation, with an yield of approxi-mately 3.9% in mass. It was further purified by DEAE-cellulose column chromatography and its chemical composi-don and in vitro anticoagulant activity was determined. The average molecular mass of the purified fucoidan wasestimated about 2.1 x 103 kDa by size-fractionation HPLC and it consisted of neutral sugar (52.34% in mass), uronicacid (26.2%), and sulfate esters (7.4%). From the HPAEC-PAD analysis, the monosaccharide composition of thepurified fucoidan was shown to be fucose, galactose, xylose, and mannose, with a molar ratio of 1, 0.2, 0.02, 0.15,respectively, demonstrating that major monosacd-iande was fucose (72.3% in mol percentage) and other sugars,xylose (1.5%), galactose (14.6%), and mannose (10.9%) were present as minor component. The results suggested thatthis fucoidan is a sulfated, U-type fucoidan. The activated partial thrombloplastin time (APTT) assay of the purifiedfucoidan showed that the purified fucoidan elicited anticoagulant activity in a dose-dependent manner. Five jUg ofsporophyll fucoidan delayed the blood clotting time up to 5 times than untreated control and also up to 1.5 timesthan the same amount of the commercial fucoidan, respectively. Although it is preliminary, these results suggestthat the fucoidan of Korean Undaria vinnatifida sporophyll would be promising candidates for the development ofan anticoaeulant.

Determination of Veterinary Antibiotic Residues: III. Analytical Methods_A Review (시료 중 잔류 항생제 분석 방법: III. 기기 분석 방법)

  • Kim, Chansik;Ryu, Hong-Duck;Chung, Eu Gene;Kim, Yongseok;Rhew, Doug Hee
    • Journal of Korean Society on Water Environment
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    • v.32 no.6
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    • pp.649-669
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    • 2016
  • This study explored the analytical conditions for 21 veterinary antibiotics which have been popularly sold in South Korea in 2014 but have not yet been targeted in EPA method 1694. Most of the selected antibiotics were separated by a reverse-phase C18 column with a combination of (buffered) water and organic polar solvent, which was commonly methanol and acetonitrile in the gradient elution mode. Volatile additives such as formic acid, ammonium acetate and ammonium formate were usually added to the mobile phases to minimize asymmetrical and tailing of antibiotics' peaks and to increase their ionization in mass spectrometry. The analytical methods of aminoglycoside antibiotics were distinct from those of the other antibiotics in terms of adoption of ion-pair chromatography (IPC) and hydrophilic interaction liquid chromatography (HILIC) capable of retaining and separating extremely polar compounds due to their hydrophilicity. Trifluoroacetic acid or heptafluorobutyric acid was frequently added to the mobile phase as an ion-pair reagent for the IPC. Tandem mass spectrometry was numerously applied to the detection of antibiotics using positive electrospray ionization (ESI) and the selected reaction monitoring (SRM) mode. All reviewed analytical methods had been/were validated by evaluating recovery, limits of detection and quantification, decision limit or detection capability of the methods.

Optimization of Extraction Conditions for Swertiamarin in Swertia japonica Makino (당약의 swertiamarin 분석을 위한 추출조건 최적화)

  • Kim, Tae Hee;Jang, Seol;Lee, Ah Reum;Lee, A Young;Choi, Goya;Kim, Ho Kyoung
    • The Korea Journal of Herbology
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    • v.29 no.1
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    • pp.13-18
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    • 2014
  • Objectives : Iridoid glycoside, swertiamarin is a well known bioactive component found in Swertia japonica Makino (SJ). In this study, we tried to optimize a suitable method which would extract swertiamarin effectively. Methods : Extraction of SJ was carried out by various conditions of time (5 - 60 min), temperature ($30-70^{\circ}C$), solvent (from non-polar to polar), and ratio of solvnet / sample (10 : 1 - 40 : 1) using ultrasonic extractor. Swertiamarin in SJ extracts was quantified by high performance liquid chromatography - Phtodiode array detector (HPLC-PDA) using C18 column and the analytical procedure was validated by evaluation of specificity, range, linearity, accuracy (recovery), precision (intra- and inter day variability), limit of detection (LOD), and limit of quantification (LOQ). Results : An efficient extraction condition for swertiamarin in SJ was optimized using sonicator extraction (temperature $40^{\circ}C$, solvent 20% methanol, solvent / sample (20 : 1), and time 10 min. Analytical procedure was optimized by HPLC-PDA using isocratic solvent system of acetonitrile and water (9 : 91), and the method was validated in regard to linearity (correlation coefficient, $R^2$ > 0.9999), range ($50-1000{\mu}g/mL$), intra- and inter-precision (RSD < 5.0 %), and recovery (99 -103 %). LOD and LOQ were 0.051 and $0.155{\mu}g/mL$, respectively. Conclusion : An optimized method of extraction for swertiamarin in SJ was established through conditions of diverse extraction and the validation result indicated that the method is suited for the determination of swertiamarin in SJ.

Seasonal Distribution of Major Copepods and Their Feeding in the Coastal Area off Taean Peninsula (태안반도 인근해역 우점 요각류의 계절별 분포와 섭식)

  • Song, Hye-Young;Lee, Doo-Byoul;Park, Chul
    • The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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    • v.15 no.4
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    • pp.149-157
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    • 2010
  • Seasonal fluctuations in abundances and ingestion rates of the three major copepods, Acartia hongi, Calanus sinicus and Paracalanus parvus s. l., around the Taean Peninsula were studied along with the estimation of the grazing impacts by them on phytoplankton standing stocks. These three copepods occupied about 50% of total mesozooplankton abundances and about 70% of total copepod abundances. A. hongi dominated in winter and spring while C. sinicus showed only one peak in spring. P parvus s. l. occurred dominantly in summer and fall. The ingestion rates of these three copepods were the highest in spring, when their abundances of eggs and nauplii were more than 10 times greater. Abundances of copepodites of these copepods were also very abundant at this time of high ingestion rates. These increased ingestion rates seemed to be related with reproduction. The grazing impacts by these three copepods were about 5% of the available chlorophyll a in the water column (with the range of 0.7 to 40.5%). The highest value was found in spring.

Determination of Amisulbrom Residues in Agricultural Commodities Using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 Amisulbrom의 잔류분석)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Kim, Min-Ji;Hwang, Young-Sun;Hong, Seung-Beom;Lee, Young Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.321-329
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    • 2014
  • This experiment was conducted to establish an analytical method for residues of amisulbrom, as recently developed an oomycete-specific fungicide showing inhibition of fungal respiration, in crops using HPLC-UVD/MS. Amisulbrom residue was extracted with acetonitrile from representative samples of five raw products which comprised apple, green pepper, kimchi cabbage, potato and hulled rice. The extract was diluted with 50 mL of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice sample, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, amisulbrom was successfully separated from sample co-extractives and sensitively quantitated by ultraviolet absorption at 255 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery test on every crop samples fortified with amisulbrom at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 85.3% to 105.6% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of amisulbrom was 0.04 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue. The proposed method was sensitive, reproducible and easy-to-operate enough to routinely determine the residue of amisulbrom in agricultural commodities.

Analytical Method for Flusulfamide as Benzenesulfonamide Fungicide, Residues in Major Agricultural Commodities (주요 농산물 중 Bezenesulfonamide계 살균제 Flusulfamide의 잔류 분석법)

  • Ahn, Kyung-Geun;Kim, Gi-Ppeum;Hwang, Young-Sun;Kang, In-Kyu;Lee, Young Deuk;Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.37 no.1
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    • pp.57-65
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    • 2018
  • BACKGROUND: An analytical method was developed using HPLC-UVD/MS to precisely determine the residue of flusulfamide, a benzenesulfonamide fungicide used to inhibit spore germination. METHODS AND RESULTS: Flusulfamide residue was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice, and soybean. The extract was diluted with large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, flusulfamide was successfully separated from co-extractives of sample, and sensitively quantitated by ultraviolet absorption at 280 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop sample fortified with flusulfamide at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries ranged from 82.3 to 98.2% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of flusulfamide was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue.