• 제목/요약/키워드: pyridine extraction

검색결과 38건 처리시간 0.028초

신 제형 클로렐라제품의 총 엽록소 시혐법 개선 (Improvement of Total Chrolophill Analytical Methods for the Chlorella Products with Extended Products Types)

  • 김유경;이은숙;한재갑;노기미;임동길;정자영;박영식
    • 한국식품위생안전성학회지
    • /
    • 제26권1호
    • /
    • pp.70-75
    • /
    • 2011
  • 본 연구에서는 새로운 제형 클로렐라제품의 정확한 총 엽록소 정량시험법을 마련하기 위해 새로운 제형 중 Syrup과 Candy 두 가지 제형의 제품을 마련하여 현행 공전방법을 적용한 함량 비교시험을 하였고 보다 정확한 결과 값을 나타낸 제1법인 pyridine 추출법의 전 처리방법을 개선하기 위하여 alkari성 pyridine으로 시료에서 엽록소를 추출하기 위하여 30분간 방치하고, 15분간 가온 할 때 초음파 처리를 병행하는 방법을 개발하여 그 결과 값의 정확성, 정밀성을 검토하였고 또 matrix sparking에 의한 정밀성과 재현성을 검토하였다. 그 결과 액상제품의 경우 pyridin 추출법과 acetone 추출법의 결과 값 CV는 18.82와 40.00, 이론치에 대한 결과 값이 106.3%와 78.1%로 상당한 차이를 보였다. Pyridin 추출법과 pyridin 추출법에 초음파 전 처리를 추가한 결과는 $27.2{\pm}5.12\;mg$/100 g와 $25.0{\pm}2.84\;mg$/100 g로 표준편차가 상당히 줄어들었고 CV도 18.82에서 11.36으로 상당히 줄어들었다. 이론치 대비율도 106.3%와 97.7%로 pyridin-초음파 추출방법이 보다 이론치에 근접한 것으로 나타났으며 회수율 측정을 하기 위하여 pyridin-초음파 추출법에 matrix spiking 한 결과도 표준편차, CV값과 이론치 대비율이 모두 향상된 결과를 나타내었다. 고형제품의 경우도 pyridin 추출법과 acetone 추출법의 결과 값 CV는 7.05와 30.00, 이론치에 대한 결과 값이 62.7%와 40%로 상당한 차이를 보였다. Pyridin 추출법과 pyridin 추출법에 초음파 전처리를 추가한 결과는 $62.7{\pm}4.42\;mg$/100 g와 $99.4{\pm}4.06\;mg$/100 g로 표준편차가 상당히 줄어들었고 CV값도 7.05에서 4.08로 상당히 줄어들었다. 이론치 대비율도 62.7%에서 99.4%로 pyridin-초음파 추출법이 명확하게 이론치에 근접한 것으로 나타났으며 회수율 측정을 하기 위하여 pyridin-초음파 추출법에 matrix spiking 한 결과도 표준편차, CV값과 이론치 대비율 모두 향상된 결괴를 나타내었다.

Fast Determination of Multiple-Reaction Intermediates for Long-Chain Dicarboxylic Acid Biotransformation by Gas Chromatography-Flame Ionization Detector

  • Cho, Yong-Han;Lee, Hye-Jin;Lee, Jung-Eun;Kim, Soo-Jung;Park, Kyungmoon;Lee, Do Yup;Park, Yong-Cheol
    • Journal of Microbiology and Biotechnology
    • /
    • 제25권5호
    • /
    • pp.704-708
    • /
    • 2015
  • For the analysis of multiple-reaction intermediates for long-chain dicarboxylic acid biotransformation, simple and reproducible methods of extraction and derivatization were developed on the basis of gas chromatography with flame ionization detector (GC-FID) instead of mass spectrometry. In the derivatization step, change of the ratio of pyridine to MSTFA from 1:3 to 9:1 resulted in higher peak intensity (p = 0.021) and reproducibility (0.6%CV) when analyzing 32 g/l ricinoleic acid (RA). Extraction of RA and ω-hydroxyundec-9-enoic acid with water containing 100 mM Tween 80 showed 90.4-99.9% relative extraction efficiency and 2-7%CV compared with those with hydrophobic ethyl acetate. In conclusion, reduction of the pyridine content and change of the extraction solvent to water with Tween 80 provided compatible derivatization and extraction methods to GC-FID-based analysis of longchain carboxylic acids.

Analyses of phenolics in cigarette smoke by GC-MS with the multiple ion selction technique

  • Park, Jeen-Woo
    • Archives of Pharmacal Research
    • /
    • 제5권2호
    • /
    • pp.71-77
    • /
    • 1982
  • Improvements in the analytical methodology used in the gas chromatographic/mass spectral analysis of phenolic compounds from cigarette smoke are described. For the direct analysis of crude samples, pyridine extraction and the glass capillary column GC was used for the separation of phenolics as trimethylsilyl derivativatives. The separations of cigarette smoke on Carbowax 20M and SE-54 wall coated open tubular columns are given. Improved methodology for the routine quantitation of the identified components using the computer-controlled multiple ion selection technique of MS presented. Considerations pertaining to routine analyses of a multitude of complex smoke samples are also discussed.

  • PDF

nPr-BTP/nitrobezene 추출 계에 의한 악티나이드(III)의 선택적 분리 (Selective Separation of Actinide(III) by a rPr-BTP/nitrobezene Extraction System)

  • 이일희;임재관;정동용;양한범;김광욱
    • 방사성폐기물학회지
    • /
    • 제6권1호
    • /
    • pp.25-33
    • /
    • 2008
  • 본 연구는 nPr-BTP/nitrobenzene 추출 계에 의한 악티나이드(III)의 선택적 분리로, 우선 자연친화적 CHN 형 의 nPr-BTP (2.6-Bis-(5.6-n-propyl-1.2.4-triazin-3-yl)-pyridine)를 합성하고, 이의 희석제에 대한 용해성 및 질산에 대한 안정성 등을 평가하였다. 악티나이드(III)의 대표원소로는 Am을 선정하였으며, 0.1M nPr-BTP/nitrobenzene-1M $HNO_3$, O/A=2의 조건에서 Am은 약 85%, RE 원소는 Eu가 8%, 기타 Nd, Ce, Y 등은 3% 이하가 추출되어 (이때 Am/Eu의 상호분리 계수 약 60정도) 악티나이드(III)의 선택적 추출에는 별 문제가 없을 것으로 판단되었다. 그러나 Am의 역추출의 경우 0.05M 질산용액으로 O/A=1 에서 약43%가 역추출 되었으며, O/A=0.3에서도 65% 정도만이 역추출 되어 질산 이외의 다른 역추출제의 개발이 요구되고 있다.

  • PDF

연속수증기증류법(SDE)과 동적헤드스페이스법(DHS)에 의한 참기름 중의 향기성분의 분석 (Analysis of Volatiles in Sesame Oil Collected by Simultaneous Distillation/Extraction(SDE) and Dynamic Headspace Sampling (DHS))

  • 하재호
    • 분석과학
    • /
    • 제9권4호
    • /
    • pp.399-405
    • /
    • 1996
  • 참기름 중의 향기성분을 연속수증기증류법(SDE)과 동적헤드스페이스법(DHS)으로 포집하여 GC와 GC-MSD로 동정하였다. SDE로 분석하였을 때 alcohol 6종, aldehyde 6종, ketone 및 acid류 5종, furan 및 phenol류 4종, pyrazine 화합물 12종, pyridine 및 thiazole류 4종, 기타 9종으로 총 46종이 확인되었다. DHS로 분석한 경우 alcohol 3종, aldehyde 6종, ketone, furan 및 phenol류 6종, pyrazine류 12종, pyridine 및 thiazole 4종, 기타 5종으로 모두 36종이 확인되었다. 대부분의 화합물이 SDE법에서 분리된 것이었으나 1-hexanol, pentanal, dimethylsulfide등은 DHS법에 의해서만 분리되었다.

  • PDF

Headspace GC-MS을 이용한 더치커피의 향기성분분석 (Studies on the Flavor Compounds of Dutch Coffee by Headspace GC-Mass)

  • 황성희;김강성;강희주;김진희;김민정
    • 한국식품조리과학회지
    • /
    • 제30권5호
    • /
    • pp.596-602
    • /
    • 2014
  • Dutch coffee is extracted in low temperature for a longer time than espresso and drip coffee. This study was conducted to investigate changes in the flavor compounds in Dutch coffee resulting from different extraction times and storage days. The fifty six flavor compounds in Dutch coffee were identified using a headspace mass-spectrometer. Major flavor compounds were 2-furfuryl acetate, 5-methylfurfural, pyridine, furfural, 2-acetylfuran, pyridine, 2-methoxyphenol, furfuryl alcohol and some compounds varied with espresso and drip coffee. It was worthy of notice that more diverse compounds were composed of total flavor in Dutch coffee. There were more kinds of flavor compounds in early extracts than in latter ones. The duration of storage didn't significantly affected the peak area percentage of flavor compounds in Dutch coffee except with 2-furfuryl acetate.

$MoH_2O_2(NCS)_3(C_5H_5N)_2$의 합성에 관한 연구 (Studies on the Synthesis of $MoH_2O_2(NCS)_3(C_5H_5N)_2$)

  • 최규원;오준석;이광우
    • 대한화학회지
    • /
    • 제7권2호
    • /
    • pp.170-173
    • /
    • 1963
  • A tri-thiocyanate molybdenum (Ⅴ) complex containing pyridine has been prepared by one step process; namely, the solvent extraction of molybdenum (Ⅴ)-thiocyanate complex into organic solvents followed by precipitation of the compound by addition of pyridine to the extract. It is concluded that the compound has a definite composition regardless of the various mole ratios of molybdenum to thiocyanate ion employed in the preparation. The use of hydrazine as the reducing agent eliminates the necessity of working under inert atmosphere and of further purification of the product. Molybdenum (Ⅴ)-thiocyanate (1:3) complex can be quantitatively and selectively extracted with slightly polar organic solvents such as ethyl acetate, and the pyridine complex is quantitatively obtained due to the insolubility of the compound in them. The oxidation state of molybdenum in the compound is + 5 and the formula appears to be $MoH_2O_2(NCS)_3Py_2$ from the contents of Mo and NCS in the compound. The solubility of the compound in various has been studied at $25^{\circ}C$.

  • PDF

Isolation of Polypeptide Fractions from Different Park offered Ginseng

  • Larina, Ludmila;Muranova, T.;Cho, B.G.;Park, H.
    • 고려인삼학회:학술대회논문집
    • /
    • 고려인삼학회 1998년도 Advances in Ginseng Research - Proceedings of the 7th International Symposium on Ginseng -
    • /
    • pp.160-167
    • /
    • 1998
  • Chemical studies of nitrogen compounds of Panax ginseng seem relatively rare, Probably due to the isolation difficulties, subsequently the investigations of biological activities are little. The experimental conditions were established for highly complete extraction of peptides (basic, acidic and neutral) from Panax ginseng. This task was achieved by applying the follow isolation procedure: 1 , the sequential extraction with water, 0.1% TFA in 20% acetonitril and buffer pH 6.5 (water-pyridine-acetic acid 100:3:900) : 2, fractionation by ultrafiltration : 3, n-butanol extraction 4, cation- and anion-exchange chromatography : 5, chromato-electrophoresis. The comparison of red ginseng (xylem Sl pith part) and red ginseng inside white (xylem Sc pith part) was also provided. To analyze the peptide mixture the chromato-electrophoresis method of separation was applied. Optimal conditions for peptides mapping of sample were explored. Our experiments revealed the quantitative difference of peptide between xylem & pith and phloem & cortex part. We have also found the qualitative difference in the composition of polypeptides between normal red ginseng (xylem Sc pith part) and red ginseng inside-white (xylem St pith part)

  • PDF

금속 chelate ion에 의한 의약품 정량에 관한 연구 (II) Dimethyglyoxime Fe(II)에 의한 Sulfa 제의 비색정량 (Studies on Drug Analysis by Metal Chelate Ion II. Colorimetric Determination of Sulfa-Drugs with Dimethylglyoxime-Fe(II))

  • 이왕규;옥치완;김박광
    • 약학회지
    • /
    • 제13권1호
    • /
    • pp.28-32
    • /
    • 1969
  • For the colorimetric determination of Sulfa-drugs by means of solvent extraction, the sample solutions were added into dimethylglyoxime-Fe(II) complex solution, and extracted with pyridine-chloroform mixture (1:50) is a range of pH 7.5-8.5. The extracted solution shows stability and maximum absorption at 402m${\mu}$.

  • PDF

금속 chelate ion에 의한 의약품 정량에 관한 연구(I) Dimethylglyoxime-Fe(II)에 의한 Nicotinamide의 비색정량 (Studies on Drug Analysis by Metal Chelate Ion. I. Colorimetric Determination of Nicotinamide with Dimethyglyoxime-Fe (II))

  • 이왕규
    • 약학회지
    • /
    • 제13권1호
    • /
    • pp.22-27
    • /
    • 1969
  • Nicotinamide Complex Compound was not formed in simple alkaline solution under two to one molar ratio of dimethyglyoxime and Fe (II), but it was formed with ammonia or pyridine under the same molar ratio. Based on this fact, nicotinamide solution was added into dimethyglyoxime-Fe (II) complex solution, and the chelation product was extracted with chloroform. The extraction was Completed in a range of pH 8.4-11.0. The chloroform solution shows stability and maximum absorption at 516 m${\mu}$.

  • PDF