• Title/Summary/Keyword: extraction solvent method

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Studies on Analysis of Food Additives- (I) Studies on the Determination of Nitrite in Foods (식품첨가물의 분석에 관한 연구 - (I) 아질산근 정량법에 관한 검토)

  • 천석조;천석조;송인상;노정배
    • Journal of Food Hygiene and Safety
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    • v.3 no.2
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    • pp.53-58
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    • 1988
  • This study was carried out to discuss a colorimetric method for the determination of nitrite in meat products issued by the Ministry of Health and Social Affaires of Korea (1985). 1) The recovery rates of nitrite of test solution extracted in the room temperature were higher than those obtained by the heating extraction. 2) In the room temperature, samples prepared with the sUce were more effective than the blendina method and the distlled water as extractina solvent for nitrite was more effective tban tbe phospbate buffer solution. 3) The extracting time showed that thirty minutes were enough to extract nitrite and the diazotizingcoupling reagents, 30% of sulfanilamide and N-l-naphthylethyienediamine were better than others. 4) The nitrite in a test soiution greatly decreased when the solution was distilled. In this case, the test solution should be used as a control. 5) Ten minutes were enough to couple nitrite.

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An Improved Method for the Determination of Scandium by Neutron Activation Analysis (스칸듐定量을 위한 改良된 放射化分析法)

  • Chung, Koo-Soon;Lee, Chul
    • Journal of the Korean Chemical Society
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    • v.8 no.2
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    • pp.88-91
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    • 1964
  • A rapid and simple method is described here for the determination of scandium in monazite by neutron activation analysis. The sample is irradiated for 20 hours at the neutron flux of $10^{12}$ thermal neutrons/$cm^2$/sec in the TRIGA MARK Ⅱ reactor, after which the sample is decomposed by fusion with concentrated sulfuric acid. The scandium-46 together with scandium carrier are separated from the irradiated sample by precipitating with ammonia, and are extracted by solvent extraction of the thiocyanate complex into ether. The induced radioactivity is measured by gamma scintillation spectrometry using the Multichannel Pulse Height Analyzer connected with 2"${\times}$2" NaI(Tl). The chemical yield is determined gravimetrically by precipitating scandium with mandelic acid. In order to check the efficiency of scandium separation and the errors from interfering activities of the other elements, scandium was separated by the cation exchange resin column, and the results from both samples were compared each other, which showed that the chemical procedure used in this work was as selective as the ion-exchange method with respect to scandium separation. The scandium contents in Korean monazite were found to be about 12 p. p. m.

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Antioxidant and Antimicrobial Activities of Camellia Oleifera Seed Oils

  • Zhou, Qing-Fen;Jia, Xue-Jing;Li, Qian-Qian;Yang, Rui-Wu;Zhang, Li;Zhou, Yong-Hong;Ding, Chun-Bang
    • Journal of Applied Biological Chemistry
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    • v.57 no.2
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    • pp.123-129
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    • 2014
  • The antioxidant and antimicrobial activities of Camellia oleifera seed oil were studied. Four kinds of seed oil samples were prepared, crude oil and refined oil, extracted by cold pressing method (CPC, CPR), and organic solvent extraction (OSC, OSR). Antioxidant activity analysis was measured in 2,2-azinobis (3-ethylbenzothiazoline-6-sulfonic acid)-diammonium salt, ferric reducing Ability of Plasma, and 2,2-diphenyl-1-picrylhydrazyl assays. Besides, the percentage of inhibition of red blood cells hemolysis induced by 2,2'-azobis(2-amidnopropane) dihydrochlorid, the lag time of LDL conjugated dienes formation in vitro, and the inhibitors of loss in tryptophan fluorescence were all used to estimate the antioxidant activity of the samples. The total phenolic contents (TPC) were detemined by Folin-Ciocalteu method. The TPC of the C. oleifera seed oils can be arranged in descending order: CPC ($1.9172{\mu}g/mL$) > OSC ($1.5218{\mu}g/mL$) > CPR ($1.0611{\mu}g/mL$) > OSR ($0.6782{\mu}g/mL$). And the oils were investigated for activity against Escherichia coli, Bacillus subtilis, Saccharomyces cerevisiae and Aspergillus niger. The results showed the antioxidant activity of crude oil by cold pressing method was stronger than others, and all oils did inhibit activity of the top three bacteria expert A. niger. The further significance of the study contributes to measure the antioxidant and antimicrobial activity of the potential health benefits by the different methods of preparation and the oil of C. oleifera seeds acting as free radical scavenger, pharmaceuticals and preservatives may offer some information in medicine and cosmetic not just in food field.

Determination of trace boron in steels by prompt gamma-ray activation analysis (즉발감마선방사화분석법에 의한 철강시료 중의 붕소 측정)

  • Kim, I.J.;Cho, K.H.;Paul, R.L.
    • Analytical Science and Technology
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    • v.22 no.4
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    • pp.302-306
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    • 2009
  • A trace amount of boron in steel significantly influences its mechanical and physical properties. A prompt gamma ray activation analysis (PGAA) method is used to measure boron in low alloy steel samples of KRISS 101-01-C21~C26. NIST SRMs of 362, 364, 1761 and 1767 serve as the control standards to validate the measurement method. The measured values of the NIST SRMs are consistent with their certified values within the expected uncertainties, except for that of NIST SRM 362. Experimental uncertainties are evaluated according to the guidelines given by the International Organization for Standardization (ISO). The expanded uncertainties are calculated with a coverage factor of 2, at approximately 95% confidence level. The calculated relative expanded uncertainties of boron mass fractions are between 3% and 7% at the mg/kg level. The results are compared with the results measured by the solvent extraction-inductively coupled optical emission spectrometry (ICP/OES) method.

Determination of Haloperidol Serum Levels in Psychiatric Patients with Gas Chromatography-Nitrogen Phosphorus Detection (GC/NPD를 이용한 정신분열증 환자의 혈중 Haloperidol 정량분석)

  • Paik, Man-Jeong;Kang, Bo-Kyoung;Lee, Kyoung-Ok;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.11 no.3
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    • pp.161-166
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    • 1998
  • Analytical method of haloperidol (HAL) in serum which has been widely used in therapy of schizophrenic disorders is developed. Gas chromatography/nitrogen-phosphorus detection (GC/NPD) was used for this study. Bromoperidol was used as an internal standard and diethylether as a solvent of three-step extraction. The extraction yield in this procedure was $67.5{\pm}1.9%$ at 15 ng/mL. A good linear response in the range of 1~40 ng/mL was obtained with correlation coefficient of $r^2=0.999$. Detection limit was 0.5 ng/mL when 2 mL of serum was used. This method was applied for the analysis of HAL in serum of schizophrenic patients. After HAL decanoate (HD) was intaken as intramuscular route, HAL levels were determined at second week and forth week. From the result, the concentration of HAL at forth week appeared to 29.6% lower than those at second week. The present method showed low detection limit and high selectivity. Therefore it can be applied for the trace analysis of HAL in serum and the monitoring.

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Gas Chromatographic and Mass Spectrometric Determination of Alcohol Homologues in the Korean Folk Sojues (Distilled Liquor) (기체크로마토그래피 및 질량분석법에 의한 민속 소주중의 알코올 동족체 분석)

  • Lee, Dong Seon;Park, Hye Seong;Kim, Geon;Lee, Taek Su;No, Bong Su
    • Journal of the Korean Chemical Society
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    • v.38 no.9
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    • pp.640-652
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    • 1994
  • This work is undertaken to determine alcohol homologues so-called fusel oil that may be present in the Korean folk sojues (distilled liquor) made from grains and to describe sample preparation and analytical method by GC-FID-MS. Solid phase extraction method for sample preparation by using porous styrene divinyl benzene polymer (Porapak Q) was compared with steam distillation and solvent extraction method. Retention behaviors of homologous series of alcohols were also studied. Log values of retention time, molecular weight, boiling point, and capacity factor of alcohols showed linear correlations to the carbon number of an alcohol, to the oven temperature, and to the dielectric constant. Components such as methyl alcohol, n-propyl alcohol, isobutyl alcohol, isopentyl alcohol, and phenethyl alcohol have been identified. The more amount of isopentyl alcohol than other alcohols are contained in the Korean folk sojues, while that of n-propyl alcohol are contained in Chinese kaoliangchiew. Degree of similarity or dissimilarity and classification of the individual samples were discussed using multivariate statistical analysis(principal components analysis) based on GC data.

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A study on the Analysis Method and Pollution Measure of existed VOCs during the Bulk Liquid Cargo Operation at Vessels (산적 액체 화물 작업중 배출되는 VOCs 분석방법 및 오염 측정 연구)

  • Cheong, Kwang-Hyun;Lee, In-Ho
    • Proceedings of KOSOMES biannual meeting
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    • 2007.05a
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    • pp.21-26
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    • 2007
  • The Protocol adopted in Sep. 1997 included the new Annex VI of MARPOL 73/78, which entered into force on 19 May 2005. Revision for the accept MARPOL Annex VI with make public on 29 Dec. 2005 and enforce on 29 Jun. 2006. For all that not installation at oil terminal or if installed do not used. The purpose of this study is to research and evaluate the methods of sampling and analysis, and the pollution measure of existed VOCs during the bulk liquid cargo operation at vessels. As the sampling instrument of VOCs, Tedlar bag has the effect of decrease in concentration by the chemical reaction and absorption, and the method using the solvent extraction has error cause because of the extraction, the absorption tube has error by the breakthrough. But canister is the best sampling instrument because of having no sampling mistake. The study on VOCs emission is not sufficient for the research on the pollution cause and the analysis data on the HAP during the bulk liquid cargo operation at vessels. Hence, monitoring on the management hazardous VOCs need to be continued during the cargo operation at vessels and VOCs management field must be study for the make progress at a good pace for reason of crew's health.

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Analysis of Glyphosate and Glufosinate in Animal Feeds using LC-MS/MS (LC-MS/MS를 이용한 동물 사료 내 글라이포세이트 및 글루포시네이트 분석)

  • Lee, Ji-Su;Kim, Wanseo;Yang, Heedeuk;Park, Na-Youn;Jung, Woong;Kim, Junghoan;Kho, Younglim
    • Journal of the Korean Chemical Society
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    • v.63 no.5
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    • pp.342-345
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    • 2019
  • The standards for the contents of glyphosate and glufosinate in foods are specific and well categorized. However, the standard of content in animal feeds is relatively inadequate and the classification is insufficient. There is also constant debate about the risk of glyphosate and glufosinate to human health, but the risk to animals has not been well studied. In this study, we established an analytical method in feeds that is estimated to be the path for animals to ingest glyphosate. The solvent extraction was carried out using 25% methanol. After centrifugation, samples were purified using solid phase extraction (SPE) and quantitatively analysed using LC-MS/MS after concentrated. Assessment of validation was conducted through detection limits, accuracy, and precision tests. The detection limits for the established method were 1.8 of ${\mu}g/kg$ of glufosinate and $2.4{\mu}g/kg$ of glyphosate. Accuracy was ranged from 94.4% to 103.4% and precision was range from 1.5% to 7.2%. Glufosinate was detected in one sample ($ND{\sim}8.8{\mu}g/kg$) and glyphosate was detected in all but one sample ($ND{\sim}337.0{\mu}g/kg$) by applying the analytical method to animal feeds (n=13).

Method Development for the Profiling Analysis of Endogenous Metabolites by Accurate-Mass Quadrupole Time-of-Flight(Q-TOF) LC/MS (LC/TOFMS를 이용한 생체시료의 내인성 대사체 분석법 개발)

  • Lee, In-Sun;Kim, Jin-Ho;Cho, Soo-Yeul;Shim, Sun-Bo;Park, Hye-Jin;Lee, Jin-Hee;Lee, Ji-Hyun;Hwang, In-Sun;Kim, Sung-Il;Lee, Jung-Hee;Cho, Su-Yeon;Choi, Don-Woong;Cho, Yang-Ha
    • Journal of Food Hygiene and Safety
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    • v.25 no.4
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    • pp.388-394
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    • 2010
  • Metabolomics aims at the comprehensive, qualitative and quantitative analysis of wide arrays of endogenous metabolites in biological samples. It has shown particular promise in the area of toxicology and drug development, functional genomics, system biology and clinical diagnosis. In this study, analytical technique of MS instrument with high resolution mass measurement, such as time-of-flight (TOF) was validated for the purpose of investigation of amino acids, sugars and fatty acids. Rat urine and serum samples were extracted by selected each solvent (50% acetonitrile, 100% acetonitrile, acetone, methanol, water, ether) extraction method. We determined the optimized liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) system and selected appropriated columns, mobile phases, fragment energy and collision energy, which could search 17 metabolites. The spectral data collected from LC/TOFMS were tested by ANOVA. Obtained with the use of LC/TOFMS technique, our results indicated that (1) MS and MS/MS parameters were optimized and most abundant product ion of each metabolite were selected to be monitorized; (2) with design of experiment analysis, methanol yielded the optimal extraction efficiency. Therefore, the results of this study are expected to be useful in the endogenous metabolite fields according to validated SOP for endogenous amino acids, sugars and fatty acids.

Analysis of gibberellic acid from fruits using HPLC/UV-vis (HPLC/UV-vis을 이용한 과일류 중의 지베렐린 산 분석)

  • Ma, Kyung Na;Cho, Hyun-Woo;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.26 no.1
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    • pp.19-26
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    • 2013
  • Gibberllic acid ($GA_3$) is one of gibberellins (GAs) that are a class of plant growth hormones that exert profound and diverse effects on plant growth and development. $GA_3$ is essentially non-UV absorbing and is difficult to assay by UV-detector. For effective extraction of gibberellic acid from fruits by using liquid-liquid extraction, optimized pH and extraction solvent were established. The selective and sensitive derivative of $GA_3$ for HPLC/UV-vis was derivatized using phenacyl bromide, and the experimental factors, including reaction time, reaction temperature and amount of derivatizing reagent and base were investigated for the effective synthesis. The derivatized $GA_3$ with phenacyl bromide was effectively analyzed by HPLC/UV-vis. The structure of derivatized $GA_3$ was confirmed by HPLC/ESI-MS. For apple, LOD and LOQ were 0.008 mg/kg and 0.027 mg/kg, respectively. For pear, LOD and LOQ were 0.003 mg/kg, 0.012 mg/kg, respectively. The established method can be applied to more effective analysis of $GA_3$ from plant and food.