• Bulletin of the Korean Chemical Society
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• 제28권10호
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• pp.1635-1636
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• 2007

• 약학회지
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• 제33권3호
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• pp.203-205
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• 1989

A method is presented for calculating the $^{13}C$ chemical shifts produced in liquid solution by referenced relative to RF frequency. The method is useful to get the real variations of chemical shifts in magnetic field by eliminating the affects of the variation of a reference substance.

• 분석과학
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• 제21권5호
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• pp.438-441
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• 2008

We have developed an alternative to the internal chemical reference based on a calibrated reference signal which is not a real NMR line but an electronically produced signal (HERETIC) and determined the phosphorus concentration using this method. The area ratio of HERETIC and sample peaks obtained from the standard samples was used to measure the concentrations of different samples directly. The analysis of phosphorus by this method showed the excellent linear regression coefficient ($R^2=0.9999$) for the concentration range from 20 ppm to 500 ppm with HERETIC peak as reference.

• 한국자기공명학회논문지
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• 제11권2호
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• pp.115-121
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• 2007

A new quantitative analysis of chloride by the HERETIC NMR method which does not need internal or external references was described. The results showed that the use of HERETIC peak corresponding $500\;{\mu}g/mL$ of chloride calibration showed less than 4 % standard deviations from 50 to $5000\;{\mu}g/mL$ range of chloride concentrations.

• 한국자기공명학회논문지
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• 제3권1호
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• pp.12-26
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• 1999

The 1H NMR signals of the heme methyl, propionate and related chemical groups of cytochrome C3 from Desulfovibrio vulgaris Miyazaki F (D.v. MF) were assigned by means of 1D NOE, 2D DQFCOSY and 2D TOCSY spectra. They were consistent with the assignments of the hemes with the highest and second-lowest redox potentials reported by Gayda et al. [Reference: 15]. The heme assignments were also supported by NOE between the methyl groups of these hemes and the side chain of Val-18, All the results contradicted the heme assignments for D.v. MF cytochrome C3 made on the basis of NMR [Reference: 11]. Based on these assignments, the interaction of cytochrome C3 with ferredoxin I was investigated by NMR. The major interaction site of cytochrome C3 was identified as the heme with the highest redox potential, which is surrounded by the highest density of positive charges. The stoichiometry and association constant were two cytochrome C3 molecules per monomer of ferredoxin I and 108 M-2 (at 53 mM ionic strength and $25^{\circ}C$), respectively.

• Elastomers and Composites
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• 제50권1호
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• pp.18-23
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• 2015

Vinyl acetate (VA) contents of poly(ethylene-co-vinyl acetate) (EVA) analyzed by infrared spectroscopy (IR), nuclear magnetic spectroscopy (NMR), and thermogravimetric analysis (TGA) were compared. Four grade EVAs supplied by Aldrich Co. and four grade EVAs manufactured by DuPont Co. were used. For IR analysis, VA contents were determined using calibration curve (absorbance ratio of $1739cm^{-1}/2922cm^{-1}$ or $609cm^{-1}/1464cm^{-1}$) of reference EVAs. Correlation coefficients of the calibration curves were not sufficiently high ($r^2{\leq}0.96$). For NMR analysis, VA contents were determined using peaks of $CH_3$, $CH_2$, and CH. VA contents determined by NMR analysis were less than those marked by suppliers more than 10%. For TGA, VA contents were determined using weight loss through deacetylation. VA contents determined by TGA were slightly different with those marked by suppliers. Difference in the VA contents determined by different analytical methods was discussed, and difference in the analytical results according to the EVA suppliers was also examined.

• 공업화학
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• 제10권1호
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• pp.160-165
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• 1999

Gel 표준 물질의 핵자기 공명적 완화 성질들이 다공성 매체내 유체의 핵자기 공명적 완화 성질들과 잘 부합될 수 있기 때문에, agarose gel은 다공성 매체내 유체의 성질을 측정하기 위한 표준 물질로 사용될 수 있다. 다공성 매체의 세공도(porosity)와 포화도(saturation)를 결정하기 위한 표준물질의 사용을 논의하였고, gel의 핵자기 공명적 성질에 대한 필요조건들도 제시하였다. 2.0 Tesla에서 측정된 agarose gel의 완화시간은 agarose 농도와 상자기성 불순물의 ($CuSO_4$) 농도 함수로 표시하였고, agarose gel 조성과 완화시간 사이의 실험적 결과를 나타내었다. 세공도 분포에 대한 평균값은 17.7%이고, 이 값은 중량 분석법에 의해 계산된 값과 잘 일치한다. 끝으로, agarose gel을 표준 물질로 사용한 비혼화성 2상 유체실험을 수행하였다. 포화 profile들은 균일한 다공성 매체내에서 일차원 치환실험을 했을 때 계산된 결과와 잘 일치하고 있다.

• 분석과학
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• 제20권5호
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• pp.400-405
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• 2007

액체크로마토그래피/질량분석법(LC/MS) 및 핵자기공명분광분석법 $^1H(NMR)$을 이용하여 화장품에 들어있는 글리세린을 동시 비교분석하였다. 화장품 시료를 물에 용해시키고 수산화나트륨을 첨가하여 시료용액을 강알칼리 상태로 유지시킨 후, 시료용액 중의 글리세린을 benzoyl chloride로 유도체화 반응 시키고 유도체화된 글리세린을 pentane으로 추출하여 LC/MS로 정량분석 하였다. $^1H$ NMR 분석은 시료를 전처리 없이 $D_2O$ 용매에 직접 용해시키고, 글리세린을 ERETIC(Electronic REference To access In vivo Concentrations) 방법을 이용하여 $^1H$ NMR로 직접 정량분석 하였다. LC/MS 및 NMR 분석결과 LC/MS의 검량선은 $0.1-10{\mu}g/mL$ 농도범위에서 $r^2=0.9991$ 이었고 $^1H$ NMR의 검량선은 $25-500{\mu}g/mL$ 농도범위에서 $r^2=1$의 상관계수를 갖는 좋은 직선성을 얻었다.

• 대한본초학회지
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• 제23권3호
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• pp.27-32
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• 2008

Objectives : In this paper, we describe that $^1H-NMR$ spectroscopy may be superior to the conventional HPLC for the quantitative analysis of hesperidin from Citrus unshiu. Methods : $^1H-NMR$ spectra (400 MHz) were recorded in $DMSO-d_6$ using a Varian UNITY Inova AS 400 FT NMR spectrometer. One hundred milligram of powdered Citrus unshiu was weighed out and mixed with 1 ml of $DMSO-d_6$ with sonication for 30 min (room temperature). The extracts were filtrated through a 0.45 ${\mu}m$ PVDF filter and 0.5 ml of filtrated extract used for quantitative $^1H-NMR$ measurement (added 1 mg of dimethyl terephthalate as internal standard). The quantity of hesperidin was calculated by the ratio of the intensity of the compound to the known amount of internal standard. For HPLC analysis, the half gram of plant material was extracted with 60 ml of MeOH for 2 hours. The extracts were made 100 ml volume and analyzed by a Waters HPLC system using a YMC ODS column. The total flow rate was 1.0 ml/min with a sample volume 10 ${\mu}l$ and UV detection at 280nm. Results : The contents of hesperidin in Citrus unshiu was determined $5.33{\pm}0.06$% in the quantitative $^1H-NMR$ method and $5.15{\pm}0.12%$ in HPLC method. Using the quantitative $^1H-NMR$ the contents of hesperidin can be determined in much shorter time than the conventional HPLC measurements. Conclusions : From those results, the advantages of quantitative $^1H-NMR$ analysis are that can be analyzed to identify and quantify, and no reference compounds required for calibration curve. Besides, it allows rapid and simple quantification for hesperidin with an analysis time for only 10 min without any pre-purification steps.

• 농약과학회지
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• 제8권2호
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• pp.88-94
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• 2004

농약제품 중 개별부자재의 확인을 위한 분석도구로서 NMR 분광기를 사용하였고 부자재의 표준품 및 농약제품을 분석 비교하였다. 고분자물질인 계면활성제는 co-polymer였고 많은 ethylene 그룹으로 이루어졌다. 가장 두드러진 signal은 긴 체인의 polyoxyethylene 그룹으로 70.5 ppm에서 나타났고 Ester의 carbnyl 그룹은 173.5 ppm에서 자기공명 signal을 확인할 수 있었다. 분석 시료는 정제, 농축, 또는 크로마토그래피의 과정 없이 준비되었고 개별부자재의 확인은 분석된 시료와 표준품 스펙트럼과의 비교에 의하여 가능할 수 있었다. NMR 분광기는 전처리과정 없이 농약제품 중 개별부자재의 분석이 가능하였다.