• Title/Summary/Keyword: 용매 분해

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Investigation of Nonylphenols Contamination in Solvents and Solid-phase Extraction Cartridge, and its Removal Protocols (정밀분석용 용매 및 SPE의 Nonylphenols 오염평가 및 제거)

  • Park, Jong-Min;Choi, Geun-Hyonng;Kim, Jung-Im;Hong, Su-Myeong;Kwon, Oh-Kyung;Im, Geon-Jae;Kim, Jin-Hyo
    • The Korean Journal of Pesticide Science
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    • v.15 no.1
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    • pp.22-27
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    • 2011
  • Nonylphenols are toxic compounds classified as endocrine disruptors. We investigated the nonylphenols clean-up procedures for the contamination control in the quantitative analysis. In this research we analyzed the residual nonylphenols in the solvent and the SPE cartridges. First, at the analysis of HPLC grade solvents (n-hexane, diethyl ether, ethyl acetate and its mixture), diethyl ether was confirmed the residue as 0.963 ${\mu}g/mL$, and we eliminated the contaminant through the distillation with $CaH_2$, Second, at the analysis of SPE cartridges (silica gel and Florisil), all products were showed the residue at 0.046~13.0 ${\mu}g/mL$, but unfortunately the residue in the cartridge were not easily removed with referenced methods in all tested SPE cartridges except in silica gel SPE cartridge with glass ware.

Analysis of General Ingredient and Amino Acid Contents in Silkworm Feces with Different Extracting Methods and Collecting Time (추출 방법 및 채취 시기를 달리한 잠분추출물의 일반성분 및 아미노산 함량 분석)

  • Sohn, Bong-Hee;Chung, Wan-Tae;Kang, Pil-Don;Ryu, Kang-Sun;Jung, I-Yeon;Kim, Yong-Soon;Kim, Kee-Young;Kim, Mi-Ja;Chung, In-Sick
    • Journal of Sericultural and Entomological Science
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    • v.49 no.2
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    • pp.43-46
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    • 2007
  • Analysis of general ingredients and amino acid content in dried silkworm feces which were extracted with hot water, EtOH, MeOH for developing new income source of rearing farm, seeking high additive value material and industrialization of silkworm feces. In the analysis of general ingredient content by extracting solution, raw protein and ash contents were increased with MeOH, EtOH, hot water. And raw fat showed higher contents by the order of EtOH > MeOH > hot water. The inorganic matter content showed a little difference among collection times of silkworm feces. Hot water was most effective extracting solution for total amino acid, and no significant difference between EtOH and MeOH. According to the time, there were no significant difference in amino acid contents. When extracted with hot water, Glu content was highest content and order of others is Asp > Gly > Ala > Leu > Thr > Ser among 18 amino acids.

Effects of Types of Catalysts and Solvents on the Water Repellency of Coating Films Prepared from MTMS and TMES (MTMS와 TMES로부터 제조된 코팅 도막의 발수성에 미치는 촉매와 용매 종류의 영향)

  • Kim, Dong Gu;Lee, Byung Wha;Song, Ki Chang
    • Korean Chemical Engineering Research
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    • v.57 no.6
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    • pp.749-757
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    • 2019
  • Methyltrimethoxysilane (MTMS) and trimethylethoxysilane (TMES) as starting materials were dissolved in various types of solvents, and hydrolysis with water and polycondensation reaction were carried out using various types of catalysts to prepare non-fluorinated water-repellent coating solutions. The coating solutions were spin-coated on cold-rolled steel sheets, and thermally cured to prepare water-repellent coating films. The effect of types of catalysts and solvents on the water repellency of the resulting coating films was investigated during this process. When hydrochloric acid and nitric acid, which are strong acids, were used as catalysts, the solutions showed a white opaque state due to the aggregation of siloxane polymers. On the other hand, when acetic acid, phosphoric acid, and oxalic acid, which are weak acids, were used, they were in a stable and transparent state without precipitation. As a result, the contact angles of the coated films, prepared from hydrochloric acid and nitric acid, were $58^{\circ}$ and $92^{\circ}$, respectively, showing low water repellency. On the other hand, when acetic acid, phosphoric acid, and oxalic acid were used, the contact angles of the coated films were $101^{\circ}$, $103^{\circ}$ and $116^{\circ}$, respectively, showing high water repellency. In addition, when isopropanol and ethanol were used as solvents, phase separation occurred in the solutions due to the aggregation of siloxane polymers. On the other hand, when methanol, ethyl acetate, and methyl ethyl ketone were used as solvents, the solutions were transparent and showed a stable state without sedimentation.

Study on Processing Methods to Remove Toxic Ptaquiloside from Bracken Fern (고사리의 독성물질 Ptaquiloside 제거방법 연구)

  • Lee, Hyang-Hee;Kim, Ae-Gyeong;Lee, Min-Gyou;Choi, Su-Yeon;Seo, Jin-Jong;Kim, Eun-Sun;Seo, Kye-Won;Cho, Bae-Sik
    • Journal of Food Hygiene and Safety
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    • v.32 no.3
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    • pp.217-221
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    • 2017
  • The ptaquiloside is a carcinogenic compound from bracken fern (Pteridium aquilinum L). This study was to evaluate the content of ptaquiloside in bracken fern by various processing methods. The processing methods were heated and immersed time, water exchange number, and so on. Akali hydrolysis and solvent fractionation of ptaquiloside in bracken fern leads to the non-toxic and chemically stable pterosin B. The contents of pterosin B was analyzed by UPLC-MS/MS on mobile phase 3 mM ammonium acetate and methanol. The contents of total pterosin B in non-processing bracken fern in water extraction was 81.0 mg/kg and toxic ptaquiloside of them was 46.4 mg/kg. The heating time of 5 minutes removed 60% about the contents of pterosin B in the bracken fern, and two-thirds of them were already non-toxic pterosin B, namely were not transfered from ptaquiloside. Additional immersed time (12h), the pterosin B in bracken fern was 10 mg/kg, it was removed 87.6% and once every hour, water exchange times were removed 99.5% in comparison with them of untreated bracken fern and two-thirds of them were non-toxic pterosin B. To remove of ptaquiloside in bracken fern, heat, immersion, and water exchange times shall be carried out simultaneously.

Elution Behavior of Pd(II) - Isonitrosoethylacetoacetate Imine Chelates by Reversed Phase High Performance liquid Chromatography (역상 액체 크로마토그래피에 의한 Pd(II) - Isonitrosoethylacetoacetate Imine 유도체 킬레이트들의 용리 거동)

  • Kim, In-Whan;Shin, Han-Chul;Lee, Man-Ho;Yoon, Tai-Kun;Kang, Chang-Hee;Lee, Won
    • Analytical Science and Technology
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    • v.5 no.4
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    • pp.389-399
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    • 1992
  • Liquid Chromatographic behavior of Pd(II) in Isonitrosoethylacetoacetate lmine, $Pd(IEAA-NR)_2$ (R=H, $CH_3$, $C_2H_5$, $n-C_3H_7$, $C_6H_5-CH_2$, $n-C_4H_9$) chelates were investigated by reversed-phase HPLC on Micropak MCH-5 column using methanol/water as mobile phase. The optimum conditions for the separation of $Pd(IEAA-NR)_2$ chelates were examined with respect to the effect of the flow rate, sample solvent, mobile phase strength and column temperature. It wass found that metal chelates were properly eluted in an acceptable range of capacity factor value($0{\leq}log\;k^{\prime}{\leq}1$). The dependence of the logarithm of capacity factor(k') on the volume fraction of water in the binary mobile phase was examined. Also, the dependence of k' on the liquid-liquid extration distribution ratio($D_c$) in methanol-water/n-alkane extration system was investigated. Both kinds of dependence are linear, which susggests that the retention of the electroneutral metal chelate is largely due to the solvophobic effect. Standard adsorption enthalpy changes (${\Delta}H^{\circ}$) and standard adsorption entropy changes (${\Delta}S^{\circ}$) of Pd(II) Isonitrosoethylacetoacetate imine chelates on Micropak MCH-5 column were calculated by measuring capacity factor with changing temperature of the column.

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생강엑기스의 제조에 관한 연구

  • 신애자
    • Food Industry
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    • s.94
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    • pp.37-40
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    • 1988
  • 1) 본 연구에서 시료로 선정한 충남 서산산 건강(dry ginger)은 수분이 $9.4\%$, 회분이 $8.7\%$ 그리고 alcohol에 의한 추출량이 약 $9\%$이다. 이는 선진국에 채택사용하고 있는 건강의 규격기준에 의하면 양호하다. 2) Non- flavor물질의 추출을 최소화하고 특히 증류과정에서 유효성분 손실을 최소화 할 수 있고, 엑기스내의 용매 잔류량이 인체에 유해하지 않고 추출효율을 높일 수 있는 용매는 ethyl alcohol이다. 3) 널리 사용하고 있는 관류추출(percolation)의 성능을 분석하고 이의 개선방안을제시하였다. - 추출효율을 높이기 위하여 건강(dry ginger)의 입자를 작게하면 압력강하가 증대되어순환되는 용액의 유속을 제어하기가 힘들다. - 입자가 작을 시에는 유체의 흐름이chan-nelling현상을 나타낸다. - 위와 같은 조건에서는 물질 전달속도가 느리므로 추출효율을 증대시킬 수가 없다. - 따라서 percolation추출에 사용되는 건강의 입자크기는 30mesh크기 이상이어야 운전조작이 용이하나 추출효율이 낮으므로, 추출시간 6시간에 회수된 생강엑기스양은 약 $2.5\%$이다. 4) percolation추출의 단점을 보완하기 위하여 기계적교반 추출을 선택하여 다음과 같은 개선점을 찾았다. - 교반형 추출에서는 고 - 액분리시 cake 저항에서 문제가 야기되지 않는 범위까지 건강의 입자를 작게할 수 있으므로 추출효율을 크게 향상시킬 수 있었다. 즉, 작게 분쇄된 건강(30mesh통과$90\%$)을 대상으로 추출시간 3시간에 $7\%$의 회수율로 증대시켰다. 최적 운전조건은 다음과 같다. 건강시료:1kg 시료크기:-30mesh$90\%$ 용매:ethyl alcohol 3$\iota$ 교반속도:900r.p.m 추출온도:상온($15\~25^{\circ}C$) 추출시간:3시간 일차 추출조건과 동일하게 하여 얻어진 엑기스의 수율이 $2\~2.5\%$이므로 총엑기스의 수율은 건강(dry ginger)무게기준으로 $8.5\~9.5\%$이었다. 5) 교반추출의 효율이 개선되었다 하더라도 추출물의 분리가 용이하여야만 공정의 이용이 가능하다. 그러므로 교반추출후 고 - 액분리를 위하여 정압여과 장치를 이용하여 여과시 cake의 평균 비저항을 얻었으며, 이의 값은 $4.31\times10^8cm\;/\;gr$으로서 여과에는 어려움이 없다는 것을 의미한다. 따라서 추출속도와 효율이 상대적으로 우수한 교반형 추출기의 가능성을 예시할 수 있음을 알 수 있었다. 6) 추출물을 농축과정에서 휘발성 oil의 손실을 최대로 줄이기 위해서는 단순증류를 하지 말고 분별증류를 수행하여야 하며, gingerol과 같은 중요성분의 열분해 반응을 억제하기 위해서는 열전달 효율을 증대시켜 증류조작을 원활히 수행하여야 하므로, still내의 농축물을 계속 교반시켜야 하며 감압상태에서 증류온도는 $40\~50^{\circ}C$로 유지시키는 것이 가장 바람직하다. 7) Ethyl alcohol로 추출된 엑기스내의 수분이나 회분함량은 외국산 제품에 비하여 약간 낮고, 반면에 조지방 및 조단백 성분의 함량은 약간 높게 나타나고 있어 대체적으로 본 연구에서 얻어진 엑기스내의 비풍미성분(non- fla-vour component) 함량은 외국산에 비하여 많은 차이가 없다. 8) 수입 외국산에 비하여 국산엑기스(본 연구에서 ethyl alcohol로 추출)내의 무기성분등의 함량은 비교적 낮은 편이다. 9) 건강에서부터 oleoresin을 얻어 paradol을 제거시킨 후 순수한 gingerol을 분리하여 IR과 NMR로 확인한 결과, 국산건강의 엑기스에는 주로 6-gingerol이고 약간의 10-gingerol이 함유된 것으로 나타났다. 10) 순수하게 분리된 gingerol을 열분석(TGA와 DTG)한 결과 약 $75^{\circ}C$에서 gingerol의 열분해 반응이 일어남을 알수 있었다. 11) 건강 분말시료와 엑기스내의 미생물 검사 결과 건강분말에서는 세균수가 많이 존재하는 것으로 나타났으나, 이는 ethyl alcohol로 추출하는 공정 중 대부분의 균들이 사멸된 것으로 나타났다. 12) 관능적 측면에선, 본 연구에서 제조한 엑기스와 수입엑기스를 비교한 결과 생강 특유의 맛은 비슷했으나, 수입엑기스에서는 쓴맛과 톱밥냄새를 느낀다는 결과를 나타내었으며 전체적인 종합적 풍미는 국산 건강엑기스가 좋은 것으로 나타났다.

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A Study on the Elution Mechanism of Ni(II)-Isonitrosoethylacetoacetate Imine Chelates by Reversed Phase High Performance Liquid Chromatography (역상 액체 크로마토그래피에 의한 Ni(II)-Isonitrosoethylacetoacetate Imine 유도체 킬레이트의 용리 메카니즘에 관한 연구)

  • Kim In-Whan;Choi Gang-Yeol;Lee Man-Ho;Kang Chang-Hee;Lee, Won
    • Journal of the Korean Chemical Society
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    • v.36 no.5
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    • pp.697-708
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    • 1992
  • Liquid Chromatographic behavior of Ni(II) in Isonitrosoethylacetoacetate Imine(IEAA-NR), Ni(IEAA-NH)(IEAA-NR)(R = H, CH_3, C-2H_5, n-C_4H_9, C_6H_5-CH_2) chelates were investigated by reversed-phase HPLC on Micropak MCH-5 column using methanol/water as mobile phase. The optimum conditions for the separation of Ni(IEAA-NH)(IEAA-NR) chelates were examined with respect to the effect of the flow rate, sample solvent, mobile phase strength and column temperature. It was fo$und that metal chelates were properly eluted in an acceptable range of capacity factor value(0{\le}logk'{\le}1). The dependence of the logarithm of capacity factor (k') on the volume fraction of water in the binary mobile phase as well as on the liquid-liquid extraction distribution ratio (Dc) in methanol-water/n-alkane extraction system showed the good linearties, and the dependence of the logarithm of capacity factor (k') on the column temperature and on the enthalpy exhibited the good linearties, and the compensation temperature ({\beta}) from the slope was 773.47{\circ}K. It was suggested that the retention of metal chelates was largely affected by the hydrophobic effect.

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Anti-microbial Activities of Ten Lauraceae Species against Propionibacterium acnes (여드름 유발균 Propionibacterium acnes에 대한 녹나무과 10종의 항균활성)

  • Cho, Ju Sung;Chi, Lai Won;Jang, Bo Kook;Jeong, Heon Sang;Lee, Cheol Hee
    • Korean Journal of Plant Resources
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    • v.31 no.5
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    • pp.423-432
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    • 2018
  • This study was performed to develop a new natural antimicrobial materials by analyzing the effect of extracts obtained from Ten Lauraceae Species on the inhibitory activity against Propionibacterium acnes. The plant materials were collected from Wando and Jeju islands, and the antimicrobial activity of the crude extracts was examined by the agar diffusion method with different part (i.e., leaf and branch), solvents (i.e., distilled water, 80% ethanol, and 100% methanol) and at different ultrasonic extracting times (i.e., 15, 30, and 45 minutes). The control agents used were synthetic antimicrobials, methylparaben and phenoxyethanol, at concentrations of 0.4, 1, 2, and 4 mg/disc. Altogether, extracts of 10 species used in the study showed inhibitory activity, which confirmed their antimicrobial action against acnes. Among these, leaves of Laurus nobilis L. which was extracted in 80% ethanol for 45 min showed the largest clear zone (19.8 mm). Leaves of L. nobilis L., showing highest antimicrobial activities among 10 species, were successively reextracted with n-hexane, chloroform, ethylacetate and n-butanol. As a results, in all fractions except butanol, clear zone above 10 mm were formed. The ethyl acetate fraction showed the highest inhibitory activity (13.3 mm) and the inhibitory activity was significantly higher than that of crude extract (10.2 mm) and phenoxyethanol as a control (12.5 mm).

Optimization of Extraction Conditions of Polyphenolic Compounds from Apple Pomace by Response Surface Methodology (반응표면분석에 의한 사과 pomace로부터의 폴리페놀 추출조건 최적화)

  • Kim, Yoon-Sook;Kim, Ro-Sa;Moon, Ji-Hye;Ji, Joong-Ryong;Choi, Hee-Don;Park, Yong-Kon
    • Korean Journal of Food Science and Technology
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    • v.41 no.3
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    • pp.245-250
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    • 2009
  • This study examined the optimization of alcohol extraction conditions for maximizing the total polyphenols derived from apple pomace, by response surface methodology (RSM). The effects of four independent variables, including $X_1$ (ratio of solvent to sample content), $X_2$ (dipping time), $X_3$ (extraction time), and $X_4$(extraction temperature), were investigated at five levels using central composite design (CCD). $Y_1$ (yield) and $Y_2$ (total polyphenols) were chosen as dependent variables. The coefficients of determination, $R^2$, were greater than 0.900 (0.9042 and 0.9555). The results showed that the model fit was very significant (p<0.001). The optimum extraction conditions were as follows: 13.00 mL/g for the ratio of solvent to sample content, 89.02 min for dipping time, 180 min for extraction time, and $70^{\circ}C$ for extraction temperature. At these conditions, the predicted total polyphenol content was 29.68 mg catechin equiv./g.

Antioxidant and Mixture Effects of Curry Spices Extracts Obtained by Solvent Extraction (용매에 따른 카레 향신료 추출물의 항산화 효과 및 혼합효과)

  • Ahn, Chae-Kyung;Lee, Young-Chul;Yeom, Cho-Ae
    • Korean Journal of Food Science and Technology
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    • v.32 no.3
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    • pp.491-499
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    • 2000
  • This study was performed to investigate the antioxidative effects of solvent extracts of eighteen curry spices. Yields of the curry spices extracted by methanol, ethylacetate and hexane were $6.4{\sim}42.9%$, $3.9{\sim}26.2%$ and $1.6{\sim}29.2%$, respectively. Methanol, ethylacetate and hexane extracts of spices were added up to 1,500 ppm in the rice bran oil and antioxidative effects of extracts were tested by Rancimat. Induction periods of spices extracted by methanol were in the order of rosemary(33.5hr)>sage(29.1hr)>ginger(28.6hr)>turmeric(26.9hr)>nutmeg(25.8hr)>oregano(25.6hr)>thyme(25.3hr)>BHT(24.5hr)>control(22.6hr). Those of ethylacetate extracts were as follows: rosemary(43.9hr)>sage(30.9hr)>oregano(29.0hr)>thyme(27.5hr)>ginger(27.1hr)>BHT(24.5hr)>control(22.6hr). Those of hexane extracts were in the order of rosemary(47.4hr)>sage(31.4hr)>oregano(27.3hr)>ginger(25.5hr)>thyme(25.1hr)>control(22.6hr). Solvent extracts of rosemary, sage, oregano, ginger and thyme showed significant antioxidative effects. Two thousands ppm hexane-extract of rosemary was the most effective. Addition of hexane-extracts of rosemary didn't show any synergism with the hexane extracts of sage, oregano, ginger, and thyme.

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