• 제목/요약/키워드: C10-CN column

검색결과 20건 처리시간 0.013초

Identification of Actinomycins by High Performance Liquid Chromatography and Fast Atom Bombardment Mass Spectrometry

  • Cho, Seong-Eun;Goo, Yang-Mo;Kim, Kyoung-Ja
    • Archives of Pharmacal Research
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    • 제17권6호
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    • pp.424-427
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    • 1994
  • An acinomycin complex isolated from culture broth of a soil microorganism, SNUS 9305-011 has been examined by High performance liquid chromatography (HPLC). From the analysis of the fractions obtained by column chromatography of the ethyl acetate extract, three actinomycin components are confimed . The HPLC analysis is carried out with a CN-bonded nucleosil column. Comparison of the retention times of the components with those of actinomycin D, C complex, $X_{o{\beta}$, and V and suggests that they are different actinomycins. FBA mass spectra fo the coponents also shows different molecular ions from those of standards and other reported actionbmycins. The present work has demonstrated that actinomycin components can be separated by a CN-bonded HPLC column, and that ocmparison of their HPLC chormatograms with authentic smaples and information on their molecular ions can be successfully employed for indentification of actionmycins.

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Determination of Co(II) Ion as a 4-(2-Thiazolylazo)resorcinol or 5-Methyl-4-(2-thiazolylazo)resorcinol Chelate by Reversed-Phase Capillary High-Performance Liquid Chromatography

  • Chung, Yong-Soon;Chung, Won-Seog
    • Bulletin of the Korean Chemical Society
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    • 제24권12호
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    • pp.1781-1784
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    • 2003
  • Determination of Co(II) ion as a 4-(2-thiazolylazo)resorcinol(TAR) or 5-methyl-4-(2-thiazolylazo)resorcinol(5MTAR) chelate was accomplished by reversed-phase capillary high-performance liquid chromatography (RP-Capillary-HPLC) using a Vydac $C_4$ column and MeCN-water mixture as mobile phase. The effect of change in pH and MeCN percentage of the mobile phase on the retention factor, k and peak intensity were evaluated. It was found that 30% MeCN (v/v) of pH 5.60 or 7.20 was adequate as mobile phase when TAR or 5MTAR is used. Detection limit (D.L., S/N=3) in each case was $2.0\;{\times}\;10^{-7}$M (11.8 ppb) and $3.0\;{\times}\;10^{-7}$ M (17.7 ppb). The Co(II) ion in mineral and waste water was determined with the optimum column and mobile phase.

생전분(生澱粉) 자화성(資化性) 미생물(微生物)의 분리(分離)와 성질(性質)에 관(關)한 연구(硏究)(II) - Aspergillus sp. SN-871이 생산하는 생전분 분해효소의 정제 및 특성 - (Studies on the screening and properties of Raw Starch Saccharifying Microorganism(II) - Purification and characterization of raw starch-digesting enzyme from Aspergillus sp. SN-871 -)

  • 서명자;노경희
    • 한국균학회지
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    • 제15권3호
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    • pp.175-182
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    • 1987
  • 1. $(NH_4)_2SO_4$침 전, DEAE-cellulose column chromatography, CM-Sephadex C-50 및 Sephadex G-75 gel filtration에 의하여 정제된 효소는 조효소보다 18배가 높았으며 회수율은 13.40%였다. 2. 겉보기 분자량은 약 40,000dalton이었다. 3. 최적 pH와 온도는 4.0, $40^{\circ}C$일 때이며, 안정범위는 pH2.0에서 pH5.0, 온도는 $60^{\circ}C$ 이하이었다. 4. 금속이온 첨가에 의한 영향은 $10^{-2}M$ $BaCl_2$첨가시 효소활성이 증가되었으며, $10^{-2}M$ $Pb(NO_3)_2$, $K_3Fe(CN)_6$, $AgSO_4$$ZnSO_4$첨가시는 효소활성이 완전히 저해되었다. 5. 각종 유기화합물 첨가에 의한 효소의 영향은 citric acid 첨가시 효소활성이 현저히 저해되었다. 6. 기질 특이성을 보면 dextrin과 glycogen을 기질로 하였을 때는 효소활성이 증가하였으나 saccharose 첨가시에는 현저히 저하되었다. 7. COD 제거율을 측정한 결과는 67에서 68% 정도이었다.

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IDENTIFICATION AND DETERMINATION OF GINSENG SAPONINS, PROSAPOGENINS AND SAPOGENINS FROM CRUDE DRUG PREPARATIONS FOR QUALITY CONTROL

  • Choi Kang Ju;Ko Sung Ryong;Kim Seok Chang;Kim Man Wook
    • 고려인삼학회:학술대회논문집
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    • 고려인삼학회 1993년도 학술대회지
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    • pp.206-214
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    • 1993
  • Ginseng saponins have been known as main active principles and analyzed as the index components in ginseng and its products for quality control. But it is generally difficult to analyze the saponins in crude drug preparations. Saponins, Prosapogenins and sapogenins of crude drug preparation were identified by TLC and determined quantitatively by HPLC. $Prosapogemins-Rg_3\;-Rg_2\;and\;{\Delta}^{20}-prosapogenin$ were extracted with ethyl acetate from $50\%$ acetic acid hydrolyzates of saponin fractions and identified by TLC with lower phase of $CHCl_3/MeOH/H_2$ O\65:35:10. v/v)on silica gel plate, and quantified by HPLC on $Lichrosorb-NH_2$ column with $CH_3CN/H_2O(90:10,\;v/v).$ Sapogenins. panaxadiol and panaxatriol. were extracted with ethyl ether from $7\%-sulfuric$ acid hydrolyzates of saponin fractions and identified by TLC with chloroform/acetone(1 : 1 v/v) on silica gel plate. and quantified by HPLC on u - Bondapak $C^{18}$ column with $CH_3CN/MeOH/CHCl_3(83:10:7.\;v/v).$ These analyses of prosapogenins and sapogenins are more useful for quality control than those of saponins in crude drug preparations such as So - Shi - Ho - Tang(소시호탕), Sa - Kun - Ja - Tang(사군자탕), Yook - Kun - Ja - Tang(육군자탕), and In - Sam -Tang(인삼탕)

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HPLC법에 의한 2,4-디니트로플루오로벤젠을 유도체화제로 한 Streptoalloteichus hindustanus ATCC 31218 변이균의 배양액 중 네브라마이신 펙터 2,4,5,5',6, 가나마이신 A 분석 (Determination of Nebramycin Factor 2,4,5,5',6 and Kanamycin A in Fermentation Broth of Streptoalloteichus hindustanus ATCC 31218 Mutant Using 2,4-Dinitrofluorobenzene(DNFB) as a Derivatizing Agent by High Performance Liquid Chromatography)

  • 박영근;박명용;김승철;양호길
    • 약학회지
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    • 제37권1호
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    • pp.1-8
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    • 1993
  • A procedure for the high-performance liquid chromatographic determination of Nebramycin factors in fermentation broth of Streptoalloteichus hindustanus ATCC 31218 mutant was investigated using pre-column derivatization and LTV detection. The method is based on pre-column derivatization of Nebramycin factors with 2,4-dinitrofluorobenzene(DNFB) in the presence of Tris (hydroxymethyl)aminoethane. The chromatographic separation of derivatives of Nebramycin factors and unknown impurities is achieved using reversed-phase column (NOVA-PAK $C_{18}$, Waters Co.) and AcCN : H$_{2}$O : AcOH (53.0:46.5:0.5) as a mobile phase. The mixture of these derivatives were separated within 35 minutes and the optimum wavelength($\lambda_{max}$ ) of the UV detector was 353 nm. The linearity of response for derivatives of Nebramycin factors is demonstrated for concentrations up to 500 $\mu\textrm{g}$/ml and the relative standard deviation is less than 0.79%. Detection limit was 1.67 ng for the 10 $\mu\textrm{l}$ sample volume employed.

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역상 모세관-고성능 액체 크로마토그래피에 의한 코발트와 니켈 이온의 4-(2-피리딜아조)레조루신올 킬레이트로서의 분리 및 정량 (Separation and Determination of Co(II) and Ni(II) Ion as their 4-(2-Pyridylazo) resorcinol Chelates by Reversed-Phase Capillary High-Performance Liquid Chromatography)

  • 정용순;정원석
    • 대한화학회지
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    • 제47권6호
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    • pp.547-552
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    • 2003
  • 코발트와 니켈 이온을 4-(2-피리딜아조)레조루신올(PAR) 리간드와 킬레이트를 만들고 이 금속-PAR 킬레이트들을 역상 모세관 고성능 액체 크로마토그래피(RP-CpHPLC)로 분리와 정량을 하였다. 컬럼은 주로 Vydac C4 모세관 컬럼을, 이동상은 아세토니트릴(MeCN) 수용액을 사용하였다. 머무름 인자, k와 봉우리 높이에 대한 이동상의 pH와 MeCN 농도의 영향을 검토하여 분리와 정량의 최적 조건을 얻었다. 결과, 분리의 최적 이동상은 22.5% MeCN, pH 5.6이었고, Co(II) 이온의 정량은 이 조건에서 할 수 있었다. 그러나 Ni(II) 이온의 정량은 분리와 봉우리의 높이로부타 22.5% MeCN, pH 7.20이 보다 적합함을 확인하였다. 각각의 조건에서 Co(II)와 Ni(II) 이온의 검출한계(D.L., S/N=3)는 각각 $2.0{\times}10{-7}$ M(14.9 ppb)와 $1.0{\times}10{-6}$ M(59.2 ppb)였다.

옻나무 껍질에서 항산화물질의 정제와 특성 (Purification and Characterization of Antioxidant Substance from the Stem Bark of Rhus verniciflua)

  • Kim, Jung-Bae
    • 한국식품영양학회지
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    • 제14권6호
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    • pp.527-531
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    • 2001
  • 옻나무는 독성이 있는 금기물질임에도 불구하고 한국에서는 민간요법으로 옻닭 등의 가공식품 형태로 사용하여 왔다. 항산화 물질은 옻나무 껍질에 물을 가하여 추출하여 분리하였다. 물 추출물은 DEAE, CN, ODS 컬럼을 사용하여 HPLC로 정제하였다. 정제된 순수물질 안정성은 pH 3.0~6.0의 산성영역에서는 안정하였으나, pH 6.5 이상에서는 불안정하였으며, 10$0^{\circ}C$에서 5시간 열처리하여도 80%의 활성을 보였다. 항균력 실험에서는 그람양성, 음성 균주에 대하여 항균 활성이 없었다. 항산화력은 DPPH 방법으로 조사한 결과 동일한 농도에서 (20$\mu\textrm{g}$/m1) BHT, BHC 보다 좋았으나, ascorbic acid 보다 낮았다.

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Simplified HPLC Method for the Determination of Pseudoephedrine Hydrochloride from Allegra D Tablet

  • Park, Moon-Hee;Shin, In-Chul
    • Biomolecules & Therapeutics
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    • 제15권2호
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    • pp.123-126
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    • 2007
  • A sensitive, simple and highly selective liquid chromatography method of determination for extraction of pseudoephedrine hydrochloride from Allegra D tablet was developed. The chief benefit of the present method is the minimal sample preparation, as the procedure is only filtering through pore syringe filter. Two drugs (pseudoephedrine hydrochloride, fexofenadine) were separated on a C$_{18}$ column and analyzed by high performance liquid chromatography (HPLC). The method had a chromatographic run time of 8.0 min. 1 ml of pseudoephedrine hydrochloride solution (1 mg/ml) was filtered through 0.22 um pore syringe filter. 50 ul of filtering solution was injected to HPLC pump and we knew the retention time (1.85 min) of separating of pseudoephedrine hydrochloride using UV detector at 280 nm. We used C$_{18}$ column (4.6 mm${\times}$250 mm), mobile phase solution (<0.05 mol/L NaH$_2$PO$_4$, 2 ml/L H$_3$PO$_4$>/CH$_3$CN / sodium dodesyl sulfate = 60 ml / 40 ml / 1 g). We separated psedoephedrine hydrochloride at run time of 1.85 min from Allegra D tablet solution (1 mg/ml) filtered through 0.22 um pore syringe filter using UV detector at 280 nm. Flow rate was set at 1.0 ml/min and the column temperature was set at 40$^{\circ}C$. Psedoephedrine hydrochloride solution (1 mg/ml) separated from Allegra D tablet was filtered through 0.22 um pore syringe filter and injected 50 ul. We confirmed the peak of psedoephedrine hydrochloride at same retention time and the separating solution was freeze-dried. In conclusion, A simple isocratic reverse-phase HPLC method has been developed that provides excellent separation of pseudoephedrine from Allegra D tablet.

Cordyceps militaris 배양액으로부터 키틴분해효소의 분리 정제 및 그 특성 분석 (Purification and Characterization of a Chitinase in Culture Media of Cordyceps militaris(Linn.) Link.)

  • 이강협;민태진
    • 한국균학회지
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    • 제31권3호
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    • pp.168-174
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    • 2003
  • C. militaris 균사를 콜로이달 키틴이 첨가된 액체 배지에서 배양한 후 황산암모늄 분별침전, 이온 교환 및 겔 여과 크로마토그래피를 이용하여 배양액 중의 chitianse를 분리 정제하였다. 이 효소의 최적 pH와 온도는 각각 5.5와 $35^{\circ}C$이었으며 겉보기 분자량은 48.5 kDa이었고, 그 Km 값은 0.57 mM이었다. 이 효소는 $Cu^{2+},\;Mn^{2+},\;Hg^{2+},\;Zn^{2+},\;CO_{3}^{2-},\;SO_4^{2-},\;CN^-$OCN^-$ 이온에 의하여 활성이 억제되었으나, $Mg^{2+}$$K^+$ 이온에 의하여 활성이 약간 증가되었다. 또한 효소 단백질의 아미노산 잔기와 선택적으로 반응하는 무수말레인산, 무수아세트산 및 N-bromo succinimide에 의하여 84.0% 활성이 억제되어 카르복실기를 가진 아미노산 잔기가 이 효소의 활성 부위에 중요한 역할을 함을 알았다. NAG6에 의한 기질 분해 특이성 실험을 통하여 이 효소는 endo-형태의 chitinase임을 알았다.

OBSERVATIONS OF $HC_3N$ TOWARD THE SGR B2 MOLECULAR CLOUD

  • MINH Y. C.;KIM HYUN-GOO
    • 천문학회지
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    • 제31권2호
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    • pp.117-125
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    • 1998
  • We have observed the 10-9 transitions of $HC_3N$ and its $^{13}C$ substitutes ($H^{13}CCCN,\;HC^{13}CCN$, and $HCC^{13}CN$), and the vibration ally excited 12-11 ($v_r=1$) $HC_3N$ transition toward the Sgr B2 molecular cloud. The observed $HC_3N$ emission shows an elongated shape around the Principal Cloud ($\~$4.5 pc in R.A. $\times$ 7.4 pc in Decl.). The optically thin $H^{13}CCCN$ line peaks around the (N) core and we derive the total column density $N(H^{13}CCCN) = 4 {\times}10^{13} cm^{-2}$ at this position. Toward the 2' N cloud which shows the peculiar chemistry, the $HC_3N$ lines show enhancements compared to the extended envelope. The shocks of the 2' N may have resulted in the enhancement of $HC_3N$. The hot component of $HC_3N$ is strongly concentrated around the (N) core and its HPW is $\~$0.9 pc in diameter. We derive the lower limit of the abundance ratio $N(HC_3N)/N(H^{13}CCCN)$ to be larger than 40 in most regions except the (M) and (N) cores. The fractionation processes of $^{13}C $at this region may not be as effective as previously reported.

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