• 제목/요약/키워드: reference compounds

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기체-액체 크로마토그래피에서 화합물의 머무름 지표의 예측에 관한 연구 (Prediction of Retention Indices of Various Compounds in Gas-Liquid Chromatography)

  • 차기원;이덕재
    • 대한화학회지
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    • 제38권2호
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    • pp.108-121
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    • 1994
  • OV-1701 모세관 컬럼과 OV-1모세관 컬럼을 사용하여 컬럼온도 150, 180, $210^{\circ}C$에서 알칸, 방향족, 알코올, 아민, 케톤, 알데히드 및 고리 화합물의 머무름 지표값을 구하였다. 기능기에 의한 머무름 인자(GRF)와 구조변화에 따른 머무름 인자(SRF)는 기능기가 없는 비교 화합물로부터 계산하였다. f번째 기능기에 따른 $GRF_f$를 구하는 식은 $GRF_f\;=\;I_{obs}-(100Z +\sum\limits_{i{\neq}f}GRF_i+{\sum}SRF_i$)와 같다. 마찬가지로 f번째의 구조변화에 따른 $SRF_i$를 구하는 식은 $SRF_f\;=\;I_{obs}-(100Z + {\sum}GRFi + \sum\limits_{i{\neq}f}SRF_i$)와 같다. 계산된 머무름 지표값과 측정값과의 차이는 OV-1701컬럼에서는 ${\pm}2$, OV-1컬럼에서는 ${\pm}3$이내였다. 또한 온도변화에 따른 기능기와 구조변화에 따른 머무름 인자 $\Delta_{ xi}$$\Delta_{ yi}$값을 기능기가 없는 비교 화합물 로부터 계산하였다. f번째 기능기에 따른 $GRF_f$를 구하는 식은 ${\Delta}x_f$ = $\Delta'/^{\circ}C+ \sum\limits_{i{\neq}f}{\Delta}xi +{\sum}{\Delta}yi$ 와 같다. 마찬가지로 f번째의 구조변화에 따른$SRF_f$를 구하는 식은 ${\Delta}yi ={\Delta}'/^{\circ}C+{\sum}{\Delta}xi + \sum\limits_{i{\neq}f}{\Delta}yi$와 같다. 계산된 ${\Delta}xi$ 값과 측정값과의 오차는 OV-1701 컬럼에는 ${\pm}18%$, OV-1컬럼에는 ${\pm}17%$였다.

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Mass Balance Method for Purity Assessment of Organic Reference Materials: for Thermolabile Materials with LC-UV Method

  • Lee, Joonhee;Kim, Byungjoo
    • Bulletin of the Korean Chemical Society
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    • 제35권11호
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    • pp.3275-3279
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    • 2014
  • A mass balance method for purity assessment of thermolabile organic reference materials was established by combining several techniques, including liquid chromatography with UV/VIS detector (LC-UV), Karl-Fischer (K-F) Coulometry, and thermal gravimetric analysis (TGA). This method was applied to three fluoroquinolones like enrofloxacin, norfloxacin and ciprofloxacin. LC-UV was used to analyze structurally related organic impurities based on UV/VIS absorbance spectra obtained in combination with LC separation. For all three organic reference materials, the UV/VIS spectra of the separated impurities were similar to that of the major component of the corresponding materials. This indicates that the impurities are structurally related to the respective reference material sharing common chromophores. Impurities could be quantified by comparing their absorbances at the wavelength of maximum absorbance (${\lambda}_{max}$). The water contents of the reference materials were measured by K-F Coulometry by an oven-drying method. The total inorganic impurities contents were assayed from ash residues in TGA analysis with using air as a reagent gas. The final purities estimated from results of those analytical techniques were assigned as ($99.91{\pm}0.06$), ($97.09{\pm}0.17$) and ($91.85{\pm}0.17$)% (kg/kg) for enrofloxacin, norfloxacin and ciprofloxacin, respectively. The assigned final purities would be applied to the reference materials which will be used as calibrators for the certification of those compounds in matrix CRMs as starting points for the traceability of their certified values to SI units.

Efficient Ultrasound Enhance Novel Series of 2-((E)-2,3-Dihydro-2-(4-(phenylthio)phenyl)benzo[b][1,4]thiazepin-4-yl)phenol as an Antimicrobial Agent

  • Chate, Asha V.;Joshi, Ratnadeep S.;Badadhe, Pravin V.;Dabhade, Sanjay K.;Gill, Charansingh H.
    • Bulletin of the Korean Chemical Society
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    • 제32권11호
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    • pp.3887-3892
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    • 2011
  • An efficient synthesis of 1,5-Benzothiazepines via Michael addition of corresponding (E)-1-(2-hydroxyphenyl)-3-(4-(phenylthio)phenyl)prop-2-en-1-one is described under ultrasound irradiation. A series of novel 2-((E)-2,3-dihydro-2-(4-(phenylthio)phenyl)benzo[b][1,4]thiazepin-4-yl)phenol derivatives was confirmed on the basis of $^1H$ NMR, Mass, IR spectral data and Elemental analysis. The synthesized compounds were evaluated for their antimicrobial activities. Most of the compounds were found to be comparable potent than the reference standard drugs. Utilization of ultrasound irradiation, simple reaction conditions, isolation, and purification makes this manipulation very interesting from an economic and environmental perspective.

장석순(張錫純)의 약물운용(藥物運用)에 관(關)한 고찰(考察) (A Study on Jangseoksun(張錫純)'s use of Herb Remedies)

  • 마해진;정창현
    • 대한한의학원전학회지
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    • 제23권3호
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    • pp.81-101
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    • 2010
  • The results of researching Jang's use of herb remedies through his book "Uihakchungjungchamseorok(醫學衷中參西錄)" are as follows. 1. Jang Seoksun's medicine is based on "Hwangjenaegyeong(黃帝內經)", "Sanghanron(傷寒論)", "Sinnongbonchogyeong(神農本草經)". And through constant study he brought to perfection his own unique medical theory. 2. He introduced Western medicine, and united it with traditional Chinese medicine. He perfected the Chinese-Western medical theory, by Chungjungchamseo(衷中參西) which means 'roots in traditional Chinese medicine, reference in Western medicine'. 3. He thought Onbyeong(溫病) was not an independent category of disease, but included it into the category of Sanghan(傷寒). So he used modified prescription of "Sanghanron(傷寒論)" to treat Onbyeong(溫病). 4. He expanded the category of remedy uses by using various compounds, such as minerals and animal compounds. He has also developed substitute remedies.

Synthesis, Analgesic, and Anti-Inflammatory Activities of [6-(3,5-Dimethyl-4-Chloropyrazole-1-yl)-3(2H)-Pyridazinon-2-yl]Acetamides

  • Sukuroglu, Murat;Caliskanergun, Burcu;Unlu, Serdar;Sahin, M.Fethi;Kupeli, Esra;Yesilada, Erdem;Banoglu, Erden
    • Archives of Pharmacal Research
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    • 제28권5호
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    • pp.509-517
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    • 2005
  • A series of structurally diverse amide derivatives of [6-(3,5-dimethyl-4- chloro-pyrazole-1-yl)-3(2H)-pyridazinone-2-yl]acetic acid were prepared and tested for their in vivo analgesic and anti-inflammatory activity by using p-benzoquinone-induced writhing test and carrageenan induced hind paw edema model, respectively. The analgesic and anti-inflammatory activity of the compounds, 7c, 7d and 7k were found to be equipotent to aspirin (as an analygesic) and indometacin (as an anti-inflammatory drug), respectively. The other amide derivatives generally resulted in lower activity on comparision with reference compounds.

Synthesis and Antiinflammatory Activity of Novel Indazolones

  • Abouzid, Khaled-A.M.;EI-Abhar, H.S.
    • Archives of Pharmacal Research
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    • 제26권1호
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    • pp.1-8
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    • 2003
  • In this study, a series of new $N^2$ substituted 1,2-dihydro-3H-indazol-3-ones (3a-d) as well as their condensed pyrazolo, pyridazino derivatives such as pyridazino[1,2-a]indazole-6,9,11-triones (4a-h) and 3,9-dioxo-3H,9H-pyrazolo[1,2-a]indazole (7) were synthesized. The antiinflammatory activity of some synthesized compounds was determined by carrageenan-induced rat paw edema technique using diclofenac as reference drug. The pharmacological data showed that most of the tested compounds exhibited a significant long lasting antiinflammatory activity, which in the case of compound 3b was superior to that of diclofenac.

Determination of Halogen Elements in Volatile Organohalogen Compounds by the Wickbold Combustion Pretreatment Method and Ion Chromatography

  • Lee, Dong-Ho;Kwon, Soo-Han;Kim, Soo-Hwan;Lee, Sang-Hun;Min, Bum-Chan
    • Bulletin of the Korean Chemical Society
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    • 제28권1호
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    • pp.59-62
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    • 2007
  • A quantitative analysis method of halogen elements in volatile organohalogen compounds was established by the Wickbold combustion pretreatment in an enclosed system and ion chromatography. The sample pretreatment parameters of Wickbold combustion were experimentally optimized, and using the determined optimal pretreatment parameters, the reproducibility was estimated by ion chromatography. As a comparison for real samples, NIST certified reference materials (CRMs) were analyzed for the recovery efficiency and reproducibility.

지용성 Benz[cd]indole 엽산길항제의 합성 및 In Vitro 항암활성 (Synthesis of Lipophilic Benz[cd]indole Antifolates and Their Antitumor Activity In Vitro)

  • 백두종
    • 약학회지
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    • 제49권1호
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    • pp.60-67
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    • 2005
  • Nonclassical aminobenz[cd]indole antifolates 4, 5 and 6, in which the glutamic acid moiety of the classical antifolates is substituted by 2-phenylglycinamide or 3-aminobenzamide, were synthesized and their in vitro antitumor activity was evaluated. The purpose of this substitution is that the lipophilicity is enhanced due to the aromatic ring of the target compounds for the passive transport through lipid membrane of cells while the hydrogen bonding of the amide is retained in the active site of the enzyme, thymidylate synthase, where the glutamate is originally present. The target compounds were highly cytotoxic against tumor cell lines of murine and human origin with micromolar to nanomolar $IC_{50}$ values. Most effective was compound 4 ($N^6-methyl-N^6$-[4-[(${\alpha}$(S)-aminocarbonylbenzyl) aminocarbonyl]benzyl]-2,6-diaminobenz[cd]indole)with $IC_{50}$ of 2 nM against SW480, human colon adenocarcinoma cell line, which is 650-fold more potent than the reference compound 3.

Phytochemical Study of Lotus ornithopodioloides L.

  • Abdel-Kader, Maged S.;Basudan, Omer A.;Alqasoumi, Saleh I.;Abou-Shoer, Mohamed I.
    • Natural Product Sciences
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    • 제13권4호
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    • pp.317-321
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    • 2007
  • Phytochemical investigation of the aerial parts of Lotus ornithopodioloides L. resulted in the isolation of six known compounds. The structures were determined utilizing physical, chemical, spectral methods as well as direct comparison with reference materials whenever possible. The compounds were identified as: ${\beta}$-sitosterol; the two triterpenes oleanolic and betulinic acids; the two cyanogenic glycosides lotaustralin and linamarin in addition to the flavonol diglycoside kaempferitin.

수목추출물의 생리활성에 관한 연구(XIII) - 회화나무잎의 화학성분(化學成分)과 항산화(抗酸化) 활성(活性) - (Studies on Biological Activity of Wood Extractives(XIII) - Chemical Components and Antioxidative activity of the leaves of Sophora japonica -)

  • 박영기;이학주;이성숙;최돈하
    • Journal of the Korean Wood Science and Technology
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    • 제31권5호
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    • pp.43-48
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    • 2003
  • 회화나무잎에서 3종의 화합물을 단리하였으며, 기기분석 결과 hypogallic acid, kaempferol, quercetin으로 각각 동정하였다. 이들 단리 물질의 항산화 활성은 라디칼 소거능으로 측정하였으며, 항산화 활성은 100 ㎍/ml의 농도에서 각각 98.2%, 96.2% 그리고 90.2%를 나타내었고 이 중 화합물 1 (hypogallic acid)과 화합물 2 (kaempferol)의 경우는 합성 항산화제인 BHT보다 높은 항산화 활성을 나타내었다.