• Title/Summary/Keyword: Liquid Liquid Extraction

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Development of Simultaneous Analysis for Multiple Agricultural Pesticides in Raw Milk Products using GC-MS/MS (GC-MS/MS를 이용한 원유 원료 중 농약 동시분석법 확립)

  • Young Nae Choi;Yoon ho Shin;Hwangeui Cho;Jung Bok Kim
    • Journal of Food Hygiene and Safety
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    • v.38 no.6
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    • pp.420-429
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    • 2023
  • GC-MS/MS using liquid-liquid extraction (LLE) and C18 cartridges was used to identify and quantify levels of chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin and permethrin in bulk raw milk. A calibration curve spanning 10 ng/mL to 200 ng/mL was obtained with a satisfactory correlation coefficient of 0.99. The limits of detection (LOD) and limits of quantitation (LOQ) for chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin, and permethrin in the matrix ranged from 0.06 to 1.81 ng/mL and 0.19 to 6.04 ng/mL, respectively. The recoveries of 5 pesticides from spiked samples at 37.5-125 ng/mL ranged from 86.1 to 102.1%. The measurement of uncertainty of the GC-MS/MS method for these five pesticides was developed based on the analytical process and quantification. An analysis method that is easier and faster than the method specified in the Korean food standards codes for analyzing these five pesticides in raw material milk was developed. Moreover, the analytical method for chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin, and permethrin in bulk raw milk by GC-MS/MS was established.

Development of Filter Sorting Process for Cigarette Butt Recycling and Extraction of Cellulose Acetate (담배꽁초 재활용을 위한 필터 선별공정 개발 및 셀룰로오스 아세테이트의 추출)

  • Minseon Park;Minjung Jung;Noh-sup Lee;Soochul Rhee;Namhoon Lee
    • Journal of the Korea Organic Resources Recycling Association
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    • v.32 no.2
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    • pp.5-14
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    • 2024
  • A study approached the development of a process for efficiently recycling discarded cigarette butts, reported as a major source of microplastic pollution in aquatic environments. Cigarette butts were sorted to extract filters, and cellulose acetate, the raw material of the filters, was extracted to a high degree of purity. The sorting of filters from cigarette butts was conducted through both wet and dry processes, each with optimized sorting conditions. Wet stirring sorting considered factors such as solid-liquid ratio, stirring speed, and stirring temperature. The highest efficiency of wet stirring sorting, at 46.21%, was observed with a solid-liquid ratio of 1:45, stirring speed of 200 rpm, and stirring temperature of 50℃. Dry wind power sorting took into account moisture content and residence time. The filter sorting efficiency reached its peak at 57.10% with a moisture content of 20% and a residence time of 5 minutes. There was no significant difference in the recovery rate of cellulose acetate between the two sorting processes. Dry wind power sorting was deemed a more advantageous process in terms of energy and environmental considerations within the scope of this study.

Properties and Suitability of Bark Extractives from Larix leptolepsis as a Bonding Agent (낙엽송(落葉松) 수피추출물(樹皮抽出物)의 특성(特性)과 접착제화(接着劑化)의 적합성(適合性))

  • Oh, Jung Do;Ahn, Won Yung
    • Journal of Korean Society of Forest Science
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    • v.77 no.3
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    • pp.294-302
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    • 1988
  • The experiment was carried out to investigate the properties of bark extractives form Larix epilepsies and to evacuate their suitability as a bonding agent. The yield and reactivity were measured to examine the influence of temperature and time and the effect of carbonation and sulfonation. To define the possibility of practical application as wood adhesives the viscosity and gelation time were measured at 33% concentration. The results obtained were summarized as follows : 1. As the both yield and reactivity were high, extraction for 2 hours at $80^{\circ}C$ was the optimal temperature and time. 2. The highest effect achieved at 1% $Na_2CO_3$ about carbonation and 1% $Na_2SO_3$ : $NaHSO_3$ and 0.25% $Na_2SO_3$ about sulfonation. The sulfonation of 0.25% $Na_2SO_3$ increased the yield and reactivity most highly. 3. By using hot water as extraction liquid the yield was 17.2%, while the addition of 1% and 5% NaOH to the extraction liquid increased the yield to 38.6% and 44.6%, respectively. 4. Hot water extracts showed the highest reactivity(68.8%). The addition of 1% and 5% NaOH led to decrease in reactivity(49.3% and 25.8%, respectively). 5. At 33% concentration of the extracts the viscosity appeared very variable. Significantly high values of viscosity was measured in 1% NaOH solution, while very low values appeared for 5% NaOH solution. 6. The shortest gelation time was determined at pH 7 to 10 and the highest at pH 4. The use of paraformaldehyde resulted in gelation times longer than those of 37% formaldehyde solution. 7. Except the sulfonation extracts of hot water and 1% NaOH, the other extracts were found unsuitable due to high viscosity(1% NaOH extracts, sulfonation extracts) or to curing inability(5% NaOH extracts, sulfonation extracts of 5% NaOH). 8. From the three extract solutions which appeared to be suitable for use as bonding agents the hot water extracts and the sulfonation extracts of hot water were superior in extract reactivity, while the sulfonation extracts of 1% NaOH exceeded the other two extracts in extract yield.

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Effect of Oil Extraction Methods on Sterol Composition of Sesame Oil (채유방법(採油方法)이 참기름의 Sterol조성(組成)에 미치는 영향(影響))

  • Choi, Sang-Do;Kim, Hyoung-Kab
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.14 no.4
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    • pp.365-369
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    • 1985
  • In order to examine the effect of oil extraction methods on the characteristics of sesame oil, the unsaponifiable matters, fractionation sterol pattern and sterol compositions of the each fraction of the oil were compared in the oil extracted by the three different extraction methods, that is, pressure extraction of roasted seed (RTP), acetone extraction of roasted seed(RTE) and acetone extraction of raw seed(RWE). The amount of unsaponifiable in RWE oil was silghly higher as 31.8mg per 1mg drying oil than that in RTP oil of 26.1mg. Sesame oils from three different extraction methods were found to contain $0.26{\sim}0.32%$ free, $0.23{\sim}0.42%$ bound, and $0.49{\sim}0.64%$ total sterol. The content of free sterol in RWE oil was higher as 0.32% than that in RTE and RTP oil of 0.26%, and that of sterylglycoside in RTE oil was lower as 0.12% than that in RTP and RWE oil of 0.23%, but that of sterylester was a little difference. The unsaponifiable matter from fractionation sterol in sesame oil by three different extraction methods was fractionated into less polor compounds, 4,4-dimethyl-, 4-monomethyl-, 4-desmethylsterol fraction by thinlayer chromatography, and sterol composition of 4-desmethylsterol fraction was analyzed by gas liquid chromatography. The major sterols were campe-, stigma-, sito-, and ${\Delta}^5-avenasterol$, but, specially, unknown sterol(RRT:1.35) was found as $23.5{\sim}26.4%$ in total sterols, The content of sitosterol, ${\Delta}^5-avenasterol$, campesterol and stigmasterol were $59.9{\sim}60.3%,\;8.1{\sim}11%,\;16.1{\sim}18.4%,\;11.6{\sim}12.8%$ of the total sterol in free sterol fraction, $37.3{\sim}46.9,\;11.6{\sim}14.2,\;6.6{\sim}9.0$, and $6.1{\sim}8.0%$ of the total sterol in sterylglycoside fraction, $55.9{\sim}59.9,\;9.2{\sim}11.4,\;17.1{\sim}18.9$, and $11.8{\sim}13.7%$ of the total sterol in sterylester fraction, and $39.3{\sim}42.9,\;13.0{\sim}17.2,\;9.1{\sim}11.0$ and $7.4{\sim}11.5%$ of the total sterol in total sterol fraction. But the effect of oil extraction methods on sterol composition in sesame oil were hardly found.

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A Study on Qualitative and Quantitative Analysis of Major ingredients in Scutellariae radix (황금(Scutellariae radix)의 주요 성분의 정성 및 정량분석에 관한 연구)

  • Rhee, Jae-Seong;Woo, Eun Ran;Kim, Nam-Hyuk;Lee, Eun-Ju;An, Duk-Kyun;Lee, Je-Hyun;Park, Seong Kyu;Park, Ho-Koon
    • Analytical Science and Technology
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    • v.10 no.2
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    • pp.91-104
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    • 1997
  • Scutellariae radix has been used on the control of body fever as oriental medicine for thousand years. Analytical aspect for the main components of Scutellariae radix was set up improving sensitivity and resolution. The analysis of 3 different flavonoids present in Scutellariae radix-baicalin, baicalein, wogonin-was conducted by means of high performance liquid chromatography with ODS reverse phase column in conjunction with a Photo Diode Array UV detector(280nm) at $40^{\circ}C$. Mobile phase was carried out at 1mL/min, composed of acetonitrile and 0.1M phosphoric acid in the form of a gradient method. Under these circumstances the retention time for baicalin, baicalein, wogonin was 7.65, 11.65 and 14.12 minutes respectively. As a result for the efficiency on extraction of active ingredients with proposed analytical process according to it's growing districts, Sunchang in Junbuk for baicalin and Bulkyo in, Junnam for bicalein and wogonin have shown the best results. Even the extraction at room temperature was satisfactory. Among acids, 0.1M acetic acid revealed the best achievements. The mixture of acetonitrile and 0.2M phosphoric acid(75:25) has been shown the best efficiency as well as stability for the extraction of active ingredients.

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Radioactivity Analysis of $^{55}Fe\;and\;^{63}Ni$ in Dismantled Concrete (해체 콘크리트 폐기물에 포함된 $^{55}Fe$$^{63}Ni$ 방사능 분석)

  • Kang, Mun-Ja;Chung, Kun-Ho;Hong, Sang-Bum;Choi, Geun-Sik;Lee, Chang-Woo
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.5 no.1
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    • pp.19-27
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    • 2007
  • Combined method of extraction chromatography and liquid scintillation analysis was established for determinating $^{55}Fe\;and\;^{63}Ni$ radioactivity in solid samples. Activated concrete wastes generated from dismantling KRR-2 were analysed. The sequential separation including precipitation and extraction chromatography resulted in the above 90% chemical recoveries of Fe. Above 62% recoveries of Ni were obtained by this procedure exception to 43.6 and 46.5% recoveries. The seperation and counting procedure was also confirmed with spiked samples of known quantity. The measured and spiked quantity were agreed with the 3.7% and 0.7% variations in the $^{55}Fe\;and\;^{63}Ni$ experiments, respectively. The radioactivities of $^{55}Fe$ in the dismantled concretes are shown from below MDA to maximum 362 Bq/g. The radioactivities of $^{63}Ni$ in all concrete samples are below MDA. The $^{63}Ni$ doesn't exist in dismantled concretes from KRR-2. The radioactivity of $^{55}Fe$ is decreased rapidly as the sampling depth is increased from the concrete surface.

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Integral Antioxidative Capacity of Extracts by Pressurized Organic Solvent from Natural Plants in Jeju (제주 자생식물 고압용매 추출물의 통합적 항산화 능력)

  • Kim, Mi-Bo;Hyun, Sun-Hee;Park, Jae-Sung;Kang, Mi-Ae;Ko, Young-Hwan;Lim, Sang-Bin
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.37 no.11
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    • pp.1491-1496
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    • 2008
  • Twenty natural plants from Jeju were extracted by pressurized organic solvent (100% methanol, $40^{\circ}C$, 13.6 MPa, 10 min). Extraction yield, total phenolic content (TPC) and integral antioxidant capacity were measured, and each component was identified by GC/MS. Extraction yields were high as 21.8%, 21.5, 21.1, 20.7 and 20.1% in Rhus javanica, Euscaphis japonica, Alnus firma, Sapium japonicum and Sorbus alnifolia, respectively. The extracts containing high TPC (mg GAE/g of dry sample) were obtained from Malus sieboldii (68.3), Sapium japonicum (57.6), Pyrrosia lingua (56.6) and Euscaphis japonica (55.1). Integral antioxidant capacities of water-soluble substances were 598, 394, 293 and $270\;{\mu}mol$ ascorbic acid equivalent/g in Geranium thunbergii, Sapium japonicum, Cornus kousa and Rhus javanica, respectively. Integral antioxidant capacities of lipidsoluble substances were 611, 314, 296 and $242\;{\mu}mol$ trolox equivalent/g in Ardisia crenata, Ostrya japonica, Geranium thunbergii and Quercus acuta, respectively. Fifteen major peaks were identified by GC/MS from the extract of pressurized organic solvent from Sapium japonicum. Two polyphenols (gallic acid (retention time (RT) 19.7 min)) and quercetin (33.5 min)), ascorbic acid (RT 35.3 min), and several fatty acids (retention time 18.6, 21.0, 21.8, 21.9 and 23.6 min) were identified, and gallic acid was the major polyphenol component due to high peak area.

Evaluation of Extractants for Bio-butanol Extraction Fermentation Using Organic Solvents and Ionic Liquids (유기용매와 이온성액체를 이용한 바이오 부탄올 추출발효 용매 선정 평가)

  • Cho, Min-Ok;Lee, Sun-Mi;Sang, Byoung-In;Um, Young-Soon
    • KSBB Journal
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    • v.24 no.5
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    • pp.446-452
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    • 2009
  • Oleyl alcohol, butyl butyrate, and two different ionic liquids were evaluated for the extraction of butanol from culture broth without toxic effect to cells. The tested solvents showed more than 50% extraction efficiency, and oleyl alcohol was chosen as the best extractant for butanol among the used extractants with a partition coefficient of 2.89. When oleyl alcohol was used as an extractant, more than 80% of butanol was extracted in the wide range of butanol concentrations (1-20 g/L) and pH values (pH 4-5.5). In extractive fermentation using oleyl alcohol only, there was 11% more butanol production and glucose consumption when compared to that without extractive fermentation, implicating a reduced inhibitory effect of butanol due to butanol removal to the oleyl alcohol phase. In addition, oleyl alcohol did not inhibit cell growth, while a mixture of oleyl alcohol and butyl butyrate with the volume ratio of 9:1~7:3 inhibited either butanol production or cell growth significantly due to the toxicity of butyl butyrate to cells. In conclusion, oleyl alcohol can be used as an efficient and non-toxic solvent for extractive fermentation for butanol production.

Preparation and Characteristics of Mixed Fruit and Vegetable Juices (혼합과채(果菜)쥬스의 제조와 제조방법에 따른 품질특성)

  • Kim, Su-Yeun;Choi, Eon-Ho
    • Korean Journal of Food Science and Technology
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    • v.30 no.1
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    • pp.90-96
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    • 1998
  • An experiment to make mixed juices carrying the freshness and other specific characteristics of vegetables and fruits which are useful for the prevention and treatment of various diseases was attempted on the emphases of pretreatment methods, combination of fruits and vegetables, and elimination of microorganisms. Blanch in boiling water prior to extraction for green vegetables, addition of ascorbic acid during extraction for tomatoes and apples, or addition of ascorbic acid after blanch in 3% acetic acid for carrots was effective to keep colors and suspended solids in liquid extract. On the basis of sensory evaluation the extracts from tomatoes, apples. carrots. mallows, watercreses+pine needles, Angelica keiskei Koiz, jujubes and lemons were selected and mixed at the ratio of 3 : 3 : 3 : 1/2 : 1/2 : 1/2 : 1/2 : 1/5. The mixed extracts were pasteurized for 15sec at $96^{\circ}C$ or filtered through a ultramembrane filter. While the centrifuge precipitation and retentates on the membrane filter were autoclaved and combined with ultrafiltrates. The mixed juices showed $pH\;4.07{\sim}4.10$ titratable acidity $66.35{\sim}84.08$, soluble solid $7{\sim}9^0Brix$, reducing sugar $5.42{\sim}6.97%$, glucose $1.96{\sim}2.30%$, fructose $3.46{\sim}4.14%$ and high content of K, Mg and Ca. Ultrafiltration showed better quality scores in color, juice. Peroxidase and microorganisms were inactivated by thermal treatment and ultrafiltration.

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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.