• Title/Summary/Keyword: shaking extraction

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Determination of eugenol in Eugenia caryophyllata by high-performance Liquid chromatography with photodiode array detection and method validation (HPLC-PDA를 이용한 정향(Eugenia caryophyllata) 중의 eugenol 분석법 확립 및 검증)

  • Yun, Hyeong-Jun;Yun, So-Mi;Lee, Myoung-Heon;Son, Seong-Wan
    • Korean Journal of Veterinary Research
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    • v.48 no.1
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    • pp.9-16
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    • 2008
  • A method for the quantification of eugenol in the medicinal herb Clove was developed and validated. For preparation of sample solutions clove was dried at $60^{\circ}C$ for 2h and ground by mixer and extracted with 95% ethanol for shaking extraction. The elutes were analyzed by HPLC system included a reversed phase column, a isocratic mobile phase of 60% methanol and PDA detector set at 280 nm. Calibration graphs were linear with very good correlation coefficients ($r^2>0.9999$) from $0.0125~1{\mu}g/ml$. The limit of detection per sample injection ($20{\mu}l$) was $0.81ng/{\mu}l$ and limit of quantification was $2.47ng/{\mu}l$. The method showed good intra-day precision (%RSD 0.08 ~ 0.27%) and inter-day precision (%RSD 0.32 ~ 1.19%).

Investigation of Optimum Extracting Condition and Antimicrobial Activity of the Extract from the Root Bark of Morus alba (상백피 추출물의 향균력 및 최적추출조건 검토)

  • 박욱연;김영목;김신희;장동석
    • Journal of Food Hygiene and Safety
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    • v.10 no.3
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    • pp.139-145
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    • 1995
  • In order to develop a natural food preservative, the root bark of Morus alba was extracted with several solvents, and then antimicrobial activity was investigated. The optimum extracting condition for the antimicrobial substance from the sample, minimum inhibitory concentration (MIC) of the extracted substance against microorganisms were also examined. The antimicrobial activity of the ethanol extract form the sample was stronger than those of the extracts by the other solvents such as water, methanol. ethyl acetate and acetone. The optimum extracting condition for antimicrobial substance from the sample was shaking extraction twice for 5 hours at room temperature in case of 7 times of absolute ethanol added to the crushed root bark of Morus alba. The ethanol extract from the root bark of Morus alba had strong B. cereus, L. monocytogenes and S. aureus. Especially, Bacillus species was the most susceptible to the extracted substance. The ethanol extract showed antimicrobial activity against Gram negative bacteria(MIC, 160~1600 ug/ml) and yeasts(MIC, 1600 ug/ml) such as C. albicans and S. acidifaeciens. The extract also showed growth inhibition against molds such as A. niger, A. parasiticus, A versicolar and T. viride.

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Simultaneous Determination of Urinary Nicotine and Cotinine Using Gas Chromatography/Nitrogen-Selective Detection (기체 크로마토그래피/질소-선택적 검출을 이용한 소변 중 니코틴과 코티닌의 동시 분석)

  • 김희갑;박미진
    • Environmental Analysis Health and Toxicology
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    • v.16 no.4
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    • pp.181-188
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    • 2001
  • A gas chromatographic method was established for the simultaneous determination of urinary nicotine and cotinine. The analytes in basified urine containing a sufficient amount of Na$_2$S0$_4$were extracted into dichloromethane by vigorous shaking. Into the transferred organic phase was added a small amount of acidified methanol (0.5 N HCI in methanol), followed by concentrating the mixture to dryness using a mild stream of nitrogen gas. The concentrate was reconstituted with methanol and the final solution analyzed using the gas chromatograph equipped with the nitrogen-phosphorus detector. The reproducibility tests showed coefficients of variation less than 11% for both compounds. The percent recovery for both analytes ranged from 88 to 103%. The estimated method detection limits for nicotine and cotinine were 0.60 and 5.1 ng/mL, respectively. Extraction efficiencies for both nicotine and cotinine apparently declined without the addition of Na$_2$S0$_4$into the urine. Moreover, the absence of methanolic HCI in the extract resulted in almost complete evaporation of nicotine and partial loss of cotinine during the concentration process, indicating that the formation of nicotine-HCI and cotinine-HCI species is prerequisite to the suppression of the loss of both compounds.

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Application and Optimization of the IsoButoxycarbonyl Derivatization method to the Analysis of Trace Level Phenols in Environmental Samples (환경시료로부터 미량 페놀류의 분석을 위한 isoButoxycarbonyl 유도체화 분석방법 적용 및 최적화)

  • Kim, Hyub;Hong, Jong-Ki;Kim, Yong-Hwa;Kim, Kyoung-Rae
    • Environmental Analysis Health and Toxicology
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    • v.17 no.1
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    • pp.37-51
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    • 2002
  • Eleven phenols including two chlorophenols, eight alkylphenols and bisphenol A were derivatized with isobutylchloroformate to form their isobutoxycarbonyl derivatives. Standard phenol mixture was concentrated for the isobutoxycarbonyl (isoBOC) derivatization and analysed by gas chromatography/mass spectrometry (GC/MS). The recoveries of the derivatization method of alkylphenols, chlorophenols, and bisphenol A were calculated by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison; shaking and heating method. The linear detector responses were obtained in the concentration range of 5∼400 ng, with correlation coefficients varying from 0.9755∼0.9981. Recoveries of the alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison ; the US-EPA method and the isoBOC derivatization method, Eleven phenols in water samples were extracted with dichloromethane and then concentrated. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 85.1∼109.9% and 90.3∼126.6% for the US-EPA method and the isoBOC.

A Study on the Functional Characteristics of Cuscuta australis R.Brown (실새삼(Cuscuta australis R.Brown)의 기능적 특성에 관한 연구)

  • Jeong, Kap-Seop
    • Journal of the Korean Applied Science and Technology
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    • v.37 no.4
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    • pp.906-914
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    • 2020
  • To investigate the usefulness of natural plants, physicochemical characteristics, functional components and physiological activities of dodder(Cuscuta australis R.Brown) were experimented. The extraction of dodder was carried out at 60℃ in shaking bath with 10 times of distilled water for three hours. Harmful metals such as lead, cadmium and arsenic were not detected, but the content of mercury from dodder was 0.0004ppm in acceptable standards. The extraction yield was 23.45%, total content of phenolics equivalent to gallic acid was 699.8 mg/100g and total content of flavonoid equivalent to naringin was 373.8 mg/100g. 28 kinds of free amino acids were detected with the contents of 252mg/100g in the dodder extract, and the contents of anserine and sarcosine were analysed highest in all amino acids. From the comparison of physiological activities of dodder extract with those of ascorbic acid, total reducing power, electron donating ability based on DPPH radical scavenging and ferric reducing antioxidant power was equivalent to 88%, 56% and 40%, respectively, of ascorbic acid. The nitrite scavenging activity of dodder extract was 78% of ascorbic acid on pH 1.5, but the antioxidant index of dodder on perilla oil was about 4 times greater than that of ascorbic acid.

The Optimal Condition for the Production and Extraction of Monacolin K from Red-Koji (홍국으로부터의 monacolin K 생성 및 추출 최적화)

  • Kwak, Eun-Jung;Cha, Seong-Kwan;Lim, Seong-Il
    • Korean Journal of Food Science and Technology
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    • v.35 no.5
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    • pp.830-834
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    • 2003
  • The optimal condition for the production and extraction of monacolin K was reported. HPLC was used to determine monacolin K a kind of metabolite of Monascus from red-koji made of Monascus purpureus CBS 281.34. After culturing Monascus in solid and liquid media at $30^{\circ}C$ for 10 days, each of these were inoculated with soybean, wheat, barley, waxy rice, and rice and cultivated at $30^{\circ}C$ for 11 days. The production of monacolin K was the highest(0.35g/100g) when cultured with rice. The yield of monacolin K in red-koji increased with drying temperature and time according to the removal of water. Considering monacolin K content and the degree of death of Monascus, red-koji was dried at $80^{\circ}C$ for 60 min. Although monacolin K in red-koji was mostly extracted by 80% ethanol, there was no difference in monacolin K between shaking for 1 min and extraction for $0{\sim}24$ hr after sonication for 7 min. The extracted yield of monacolin K was the highest when the ratio of red-koji and 80% ethanol was 1:9. Moreover, the production of monacolin K appeared to be parallel with that of the pigment.

Antioxidant and Anti-Inflammatory Effects on Optimal Extraction Conditions of Different Edible Parts of Perilla (Perilla frutescens L.) (들깨 가식부위별 최적 추출 조건 확립을 위한 항산화 및 항염증 활성 평가)

  • Min Young Kim;Jung In Kim;Sang Woo Kim;Sungup Kim;Eunyoung Oh;Jeongeun Lee;Eunsoo Lee;Yeon Ju An;Myoung Hee Lee;Choon-Song Kim
    • The Korean Journal of Food And Nutrition
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    • v.36 no.6
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    • pp.551-560
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    • 2023
  • This study was performed to investigate antioxidant and anti-inflammatory activities of perilla(Perilla frutescens L.) seed, flower and leaf according to extraction condition. Perilla seed extracts(PSE), perilla flower extracts(PFE), perilla leaf extracts(PLE) was extracted by stirring extraction (STE, 25℃), shaking extraction (SHE, 80℃), and sonication assisted extraction(SAE, 25℃) with 94% ethanol, 60% ethanol and distilled water, followed by analysis of total polyphenol and flavonoid and testing radical scavenging activities. The highest total polyphenol content (5.47, 9.36, 38.58 mg gallic acid equivalent/g), total flavonoid content(5.77, 8.62, 46.44 mg catechin equivalent/g), ABTS(10.68, 19.46, 63.56 mg trolox equivalent/g) and DPPH(6.51, 7.69, 79.73 mg trolox equivalent/g) radical scavenging activity of PSE, PFE and PLE was observed in the HWE with 60% ethanol,. Among the three extraction method, SHE provided the best results for yield, polyphenol, flavonoid content of perilla seed, flower, leaf in comparison to STE or SAE. SHE with 60% ethanol of perilla seed, flower, leaf more effectively inhibited secretion of nitric oxide(NO) and pro-inflammatory cytokine in RAW 264.7 macrophage exposed to LPS compared to other extraction solvent and method. Therefore, these extracts obtained from perilla seed, flower, leaf could be used antioxidant and anti-inflammatory ingredients in the food industry.

A Method for Simultaneous Analysis of Phthalate Esters and Di-(2-ethylhexyl) Adipate Migrated from PVC Wraps into Fatty Food (PVC Wraps에서 지방함유 식품으로 이행되는 Phthalate esters 및 Di-(2-ethylhexyl) adipate의 동시 분석법)

  • Lee, Kwang-Ho;Jeon, Dae-Hoon;Jeong, Dong-Youn;Choi, Byung-Hee;Kim, Sung-Wook;Lee, Chul-Won
    • Korean Journal of Food Science and Technology
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    • v.32 no.6
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    • pp.1244-1250
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    • 2000
  • A method for simultaneous quantitative determination of plasticizers such as diethyl phthalate(DEP), di-n-propyl phthalate(DprP), di-n-butyl phthalate(DBP), di-n-pentyl phthalate(DPP), butylbenzyl phthalate(BBP), di-(2-ethylhexyl) phthalate(DEHP), dicyclohexyl phthalate(DCHP) and di-(2-ethylhexyl) adipate(DEHA), which are suspected as endocrine disruptors, in food was studied. A analysis method was optimized for the quantification of plasticizers in Jjambbong, which is a kind of fatty noodle, by using GC/FID. The detection limits of DEP, DprP, DBP, DPP, BBP, DEHP, DCHP and DEHA were 3.5, 5.3, 2.2, 2.2, 7.2, 1.7, 1.9 and 3.0 mg/kg, respectively. Much higher recovery was obtained by extraction with acetone/n-hexane(1:1) rather than hexane solvent system. The recovery of DEP, DprP, DBP, DPP, BBP, DEHP, DCHP and DEHA were 72.7, 85.9, 91.4, 97.1, 100.8, 103.2, 104.3 and 95.8% after 4 time extractions, respectively. The migration of plasticizers from PVC wraps into PVC wrap covered Jjambbong was conducted after shaking(120 rpm) for 30min at room temperature with chosen solvent system. It was found that the migration level of DEHA were 577, 706, 770 mg/kg into Jjambbong, respectively, while the other plasticizers were not observed.

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Derivation of Dynamic Characteristic Values for Multi-degree-of-freedom Frame Structures based on Frequency Response Function(FRF) (주파수응답함수 기반 다자유도 골조 구조물의 동특성치 도출 및 구조모델링 적용 )

  • So-Yeon Kim;Min-Young Kim;Seung-Jae Lee;Kyoung-Kyu Choi
    • Journal of the Korea institute for structural maintenance and inspection
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    • v.27 no.4
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    • pp.1-10
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    • 2023
  • In the seismic design of structures, seismic forces are calculated based on structural models and analysis. In order to accurately address the dynamic characteristics of the actual structure in the structural model, calibration based on actual measurements is required. In this study, a 4-story frame test specimen was manufactured to simulate frame building, accelerometers were attached at each floor, and 1-axis shaking table test was performed. The natural period of the specimen was similar to that of the actual 4 story frame building, and the columns were designed to behave with double-curvature having the infinite stiffness of the horizontal members. To investigate the effects seismic waves characteristics, historical and artificial excitations with various frequencies and acceleration magnitudes were applied. The natural frequencies, damping ratios, and mode shapes were obtained using frequency response functions obtained from dynamic response signals, and the mode vector deviations according to the input seismic waves were verified using the Mode assurance criterion (MAC). In addition, the damping ratios obtained from the vibration tests were applied to the structural model, and the method with refined dynamic characteristics was validated by comparing the analysis results with the experimental data.

Studies on Solvent Extraction and Analytical Application of Metal-dithizone Complexes(I). Separation and Determination of Trace Heavy Metals in Urine (Dithizone 금속착물의 용매추출 및 분석적 응용(제1보). 뇨중 흔적량 중금속 원소의 분리 정량)

  • Jeon, Moon-Kyo;Choi, Jong-Moon;Kim, Young-Sang
    • Analytical Science and Technology
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    • v.9 no.4
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    • pp.336-344
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    • 1996
  • The extraction of trace cobalt, copper, nickel, cadmium, lead and zinc in urine samples of organic and alkali metal matrix into chloroform by the complex with a dithizone was studied for graphite furnace AAS determination. Various experimental conditions such as the pretreatment of urine, the pH of sample solution, and dithizone concentration in a solvent were optimized for the effective extraction, and some essential conditions were also studied for the back-extraction and digestion as well. All organic materials in 100 mL urine were destructed by the digestion with conc. $HNO_3$ 30 mL and 30% $H_2O_2$ 50 mL. Here, $H_2O_2$ was added dropwise with each 5.0 mL, serially. Analytes were extracted into 15.0 mL chloroform of 0.1% dithizone from the digested urine at pH 8.0 by shaking for 90 minutes. The pH was adjusted with a commercial buffer solution. Among analytes, cadmium, lead and zinc were back-extracted to 10.00 mL of 0.2 M $HNO_3$ from the solvent for the determination, and after the organic solvent was evaporated, others were dissolved with $HNO_3-H_2O_2$ and diluted to 10.00 mL with a deionized water. Synthetic digested urines were used to obtain optimum conditions and to plot calibration-eurves. Average recoveries of 77 to 109% for each element were obtained in sample solutions in which given amounts of analytes were added, and detection limits were Cd 0.09, Pb 0.59, Zn 0.18, Co 0.24, Cu 1.3 and Ni 1.7 ng/mL, respectively. It was concluded that this method could be applied for the determination of heavy elements in urine samples without any interferences of organic materials and major alkaline elements.

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