• Title/Summary/Keyword: solvent recovery

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Simultaneous Determination and Optimization Ultrasound-Assisted Extraction of Poncirin and Naringin in Poncirus trifoliata Rafinesqul (지실의 Poncirin, Naringin의 동시분석법 확립과 초음파 추출법 최적화)

  • Lee, Ah Reum;Jang, Seol;Lee, A Yeong;Choi, Goya;Kim, Hyo Seon;Kim, Ho Kyoung
    • Korean Journal of Medicinal Crop Science
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    • v.22 no.2
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    • pp.147-153
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    • 2014
  • The Ponciri fructus immaturus (Poncirus trifoliata Rafinesque) has been used in oriental medicine for uterine contraction, stomachache, abdominal distension and cardiovascular diseases. Two main compounds, poncirin and naringin were successfully analyzed by high performance liquid chromatography (HPLC) and carried out method validation according to ICH guideline. A successful resolution and retention times were obtained with a $C_{18}$ reversed phase column, at an $1m{\ell}min^{-1}$ flow rate, with a gradient elution of a mixture of methanol, water and acetonitrile. Poncirin and naringin showed good linearity ($R^2$ > 0.999) in relatively wide concentration ranged. The recovery of each compound was 95.81 ~ 101.48% with R.S.D. values less than 1.0%. The application of ultrasound-assisted extraction was shown to be more efficient in extracting poncirin and naringin from Ponciri fructus immaturus. The predicted optimal poncirin and naringin yield were poncirin 2.15%, naringin 1.65% under an extraction temperature of $40^{\circ}C$, an extraction time of 10 min in a solvent of 70% methanol.

Determination of Polybrominated Biphenyls in Biota Samples Using Gas Chromatography/Mass Spectrometry (기체크로마토그래피/질량분석법을 이용한 생체시료 중 Polybrominated Biphenyls의 분석법)

  • Hong, Jongki;Baek, In-Girl;Kim, Hyub;Kim, Do-Gyun;Seo, Jung-Joo;Seo, Jong-Bok;Park, Hyun-Mee;Lee, Kang-Bong
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.666-674
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    • 2000
  • The present study describes an analytical method for the determination of polybrominated biphenyls (PBBs) in biota samples by gas chromatography-mass spectrometry (GC/MS). PBBs are extracted twice from 20 g samples with mixture solvent 40mL acetone and 80mL hexane using ultrasonic agitation for 20 min. Lipids in extracts are degraded by concentrated sulfuric acid and then PBBs are purified with Florisil column. The purified extracts are analyzed by GC/MS-selected ion monitoring mode for the quantitation of PBBs in biota sample. The overall recovery yields of PBBs range between 77 and 111% under these experimental conditions.

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한국산(韓國産) 광대싸리(Securinega suffruticosa Rehder)에서의 Securinine 추출(抽出)

  • Lee, Chun-Yeong;Lee, Seong-Hwan;An, Hak-Su
    • Applied Biological Chemistry
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    • v.6
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    • pp.33-36
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    • 1965
  • 1. The extraction of securine, an alkaloid, from Securinega suffruticosa Rehder growing in Korea was investigated. 2. The distribution of the source plant in Korea is considered to be most intense among the Fareast countries. 3. The extracted material was identified to be genuine securinine viewing from melting point and microscopic observation. 4. The yield of the substance in this study was 0.075% in average. The less amount of recovery may be due to the collection of the plant in October instead of that in the prime season. 5. There should be more efficient way in the separation of resinous impurities from the crude product. Application of Chromatographic technique and selection of more efficient solvent will be investigated hereafter.

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Determination of Cadmium(II) and Copper(II) by Flame Atomic Absorption Spectrometry after Preconcentration on Column with Pulverized Amberlite XAD-4 with Bismuthiol I

  • Park, Dong-Seok;Choi, Hee-Seon
    • Bulletin of the Korean Chemical Society
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    • v.28 no.8
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    • pp.1375-1382
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    • 2007
  • A column preconcentration method with pulverized Amberlite XAD-4 loaded with bismuthiol I (BI) has been developed for the determination of trace Cd(II) and Cu(II) in various real samples by flame atomic absorption spectrophotometry. Various experimental conditions, such as the size of XAD-4, adsorption flow rate, amount of bismuthiol I, stirring time for adsorbing bismuthiol I on XAD-4, pH of sample solution, amount of XAD-4- BI, desorption solvent, and desorption flow rate, were optimized. Also, the adsorption capacity and the adsorption rate of Cd(II) and Cu(II) on XAD-4-BI were investigated. The interfering effects of various concomitant ions were investigated, Bi(III), Sn(II) and Fe(III) were found to affect the determination. But the interference by these ions was completely eliminated by adjusting the amount of XAD-4-BI resin to 0.70 g, although the adsorption flow rate was slower. For Cd(II) our proposed technique obtained a dynamic range of 0.5-40 ng mL-1, a correlation coefficient (R2) of 0.9913, and a detection limit of 0.3 ng mL-1. For Cu(II), the corresponding values were 2.0-120 ng mL-1, 0.9921 and 1.02 ng mL-1. To validate this proposed technique, the aqueous samples (stream water, reservoir water, tap water and wastewater), the diluted brass sample and the plastic sample, as real samples, were used. Recovery yields of 91-103% were obtained. These measured data were not different from ICP-MS data at 95% confidence level. Our proposed method was also validated using rice flour CRM (normal, fortified) samples. From the results of our experiment, we found that the technique we present here can be applied to the determination of Cd(II) and Cu(II) in various real samples.

Simultaneous Determination of Various Pesticides (I): Analysis by GC with ECD and NPD Dual Detectors (잔류농약 다성분 동시분석법에 관한 연구(I): GC-ECD 및 NPD를 병렬 사용한 분석)

  • Rho, Kyoung-Ah;Kim, Jin-Ho;Kim, Hyeon-Wee;Lee, Yoon-Kyoung;Park, Ki-Moon
    • Korean Journal of Food Science and Technology
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    • v.29 no.3
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    • pp.427-431
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    • 1997
  • A simultaneous and rapid gas chromatographic determination of organophosphorus, organo-chlorine, carbamate, and pyrethroid pesticides in polished rice was developed. The pesticides were extracted from samples with acetone by automated soxhlet apparatus and this extract was evaporated to dryness. The residue was dissolved in hexane, the solvent was applied to a Sep-Pak florisil catridge, was eluted with 50% ethyl acetate in n-hexane, and was injected to dual GC-ECD/NPD system. This simple method affords a high recovery of hydrophilic pesticides, allows rapid analysis, and is cheap to perform. Except for dichlorvos and captan, recoveries of 46 pesticides were over 60%.

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Beta-carotene and Lutein Contents in Green Leafy Vegetables (녹색잎 채소류의 ${\beta}$-Carotene과 Lutein 함량)

  • Lee, Hwa-Suk;Kim, Young-Nam
    • Journal of the East Asian Society of Dietary Life
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    • v.7 no.2
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    • pp.175-180
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    • 1997
  • Beta-carotene and lutein contents in 7 different green leafy vegetables(perilla leaf, mugwort, chwi, lettuce, spinach, leek, and crown daisy) were analyzed by HPLC. The isocratic separation was performed on a ${\mu}-Bondapak$ $C_{18}$ column with a solvent system of acetonitrile : dichloromethane : methanol = 70:20:10. To check the reliability of the method applied, precision and recovery tests were performed. Perilla leaf showed the highest ${\beta}-carotene$ content(12,570 ${\mu}g$ / 100 g), followed by mugwort and chwi, all of those have ${\le}10,000\{\mu}g\{\beta}-carotene$ per 100 g vegetables. Green lettuce, spinach, leek, crown daisy and reddish brown lettuce contained 9,869, 6,689, 5,664, 3,601 and 3,299 ${\mu}g\{\beta}-carotene/100 g$, respectively, Lutein content was the highest in perilla leaf($13,718{\mu}g/100 g$) followed by chwi($11,989{\mu}g/100 g$), mugwort($11,522{\mu}g/100 g$), green lettuce($10,307{\mu}g/100 g$) and spinach($10,115{\mu}g/100 g$). ${\beta}-carotene$ contents in perilla leaf, mugwort, chwi and green lettuce were 47.8~49.6% of total carotenoids, and ${\beta}-carotene$ contents in the other green leafy vegetables analyzed were 37.7~41.4% Vitamin A contents of green leafy vegetables analyzed by HPLC were 2~6 times higher than the vitamin A values shown in food composition tables except crown daisy.

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Recovery of Cu and Sn from the Bioleaching Solution of Electronic Scrap (전자(電子)스크랩의 미생물(微生物) 침출액(浸出液)으로부터 구리 및 주석의 회수(回收)에 관한 연구(硏究))

  • Ahn, Jae-Woo;Kim, Meong-Woon;Jeong, Jin-Ki;Lee, Jae-Chun
    • Resources Recycling
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    • v.15 no.6 s.74
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    • pp.41-47
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    • 2006
  • A study for recovering of copper and lead from electronic scraps has been carried out using a combination of bioleaching and solvent extraction. It was found that the citric acid generated by Aspergillus niger could be an imporant leaching agent acting in the solubilization of copper, iron, lead and tin from the electronic scrap. Copper could be selectively extracted by 10% LIX84 from the leaching solution and it recoved 99.9% of metallic copper by electrowinning process. Tin and iron were extracted from the remaining solution by 10% Alamine336 and stripped by NaCl solution. Finally, tin could be recovered as a metallic precipitates from the mixed solution of tin and iron by cementation with iron powder.

Polyaniline/SiO2 Catalyzed One-pot Mannich Reaction: An Efficient Synthesis of β-amino Carbonyl Compounds (Polyaniline/SiO2를 이용한 one-pot Mannich 반응: β-amino carbonyl 화합물의 효율적인 합성)

  • Yelwande, Ajeet A.;Arbad, Balasaheb R.;Lande, Machhindra K.
    • Journal of the Korean Chemical Society
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    • v.55 no.4
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    • pp.644-649
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    • 2011
  • Polyaniline/$SiO_2$ catalyzed one-pot mannich reaction of acetophenone, aromatic aldehydes and aromatic amines are carried out in ethanol to afford various ${\beta}$-amino ketones. The various wt% of polyaniline were supported on pure silica synthesized by using chemical oxidative method. The catalyst prepared has been characterized by means of thermal analysis (TG-DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM) energy dispersive spectroscopy (EDS), and Fourier transform infrared spectroscopy (FT-IR). Solvent stability of catalyst was tested using UV-Visible spectroscopy. This protocol has several advantages such as high yield, simple work up procedure, non-toxic, clean, easy recovery and reusability of the catalyst.

Analytical Determination of Alkylphenols, Chlorophenols and Bisphenol A in Biota Samples using Gas Chromatography/Mass Spectrometry (기체 크로마토그래피/질량분석기를 이용한 생물시료 중 알킬 페놀류, 클로로페놀류 및 비스페놀 A의 분석법)

  • Hong, Jongki;Kim, Hyup;Baek, In-Girl;Kim, Do-Gyun;Seo, Jung-Joo;Seo, Jong-Bok;Chung, Bong-Chul;Pyo, Hee-Soo;Kim, Kyung-Rae;Kim, Yong-Hwa
    • Analytical Science and Technology
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    • v.13 no.4
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    • pp.484-493
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    • 2000
  • The simultaneous analysis of alkylphenols, chlorophenols and bisphenol A in biota samples was performed by gas chromatography-mass spectrometry-selected ion monitoring mode. The phenols were extracted from sample with organic solvent and Forisil and Silica columns for clean-up procedure were compared. Recovery studies were performed at 1-ppm level of phenols added to each biota sample. Their recoveries ranged between 83 and 116% with coefficient of variations of 2.4-11.9%. To improve the detection limits of phenols, trimethylsilyl (TMS) derivatization was applied. The gas chromatographic properties of free phenols and TMS derivatized phenols were also investigated.

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Method Validation and Uncertainty Estimation for Toluene Measurement in Biological Fluids by HS-GC (HS-GC에 의한 생체 시료내 톨루엔 분석에 대한 방법의 유효화와 불확도 추정)

  • Heo, Sangcheol;Min, Ji-Sook;Park, Jongseo;Lim, Mi-Ae;Park, Sungwoo
    • Analytical Science and Technology
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    • v.17 no.6
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    • pp.443-453
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    • 2004
  • Toluene is currently used as a major organic solvent of glues which are abused by the youngster for its hallucinogenic effect. In this study, toluene determination method using headspace gas chromatography (HS-GC) in the biological fluids like blood, urine and saliva of glue sniffers was validated and related uncertainties were estimated. LOD of $0.01{\mu}g/mL$ in saliva and LOQ of $0.1{\mu}g/mL$ in blood were the highest among LODs and LOQs in urine, blood and saliva. Other performance characteristics such as linearity, working range, accuracy, precision and recovery were also measured. The uncertainty at toluene concentration of $1{\mu}g/mL$ was estimated to be 0.13, 0.09 and $0.17{\mu}g/mL$ for blood, urine and saliva, respectively, and the uncertainty contribution from the least linear regression was dominant at the lower concentration of toluene.