• 생약학회지
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• 제47권3호
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• pp.232-236
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• 2016

In traditional Korean medicine, Osmunda japonica Thunb has been used as hemostasis and antipyretic treatment. The main compound "cinnamtannin B-1" was obtained by column chromatographic separation, and its structure was determined by spectroscopic methods, including $^1H$, $^{13}C$ NMR, and IT-TOF-ESI MS. Ash, moisture and extract content and acidinsoluble ash were monitored as identification test to establish the analytical methods. The optimum reflux extraction condition was 100% methanol extracted 30 min for 2 times. A quantitative analysis using HPLC method exhibited that the main compound at 24.7 min and its content was 0.96% in methanol extraction.

• 약학회지
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• 제56권5호
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• pp.280-287
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• 2012

A high-performance liquid chromatography (HPLC) combined with ultraviolet (UV) method for the simultaneous determination of ${\alpha}$-cyperone and nootkatone was developed for the quality control of Cyperus rotundus Linne. The separation was performed on a KR100-$5C_{18}$ ($4.6{\times}250mm$) column, and an elution gradient composed of methanol and water with a flow-rate of 1.0 ml/min. Detection wavelength was set at 254 nm. The optimum extraction for the detection of the ${\alpha}$-cyperone and nookatone was achieved by ultrasonic with methanol for an hour. Two marker compounds ${\alpha}$-cyperone and nootkatone in Cyperi Rhizoma showed good linearity ($R^2$ >0.999) in the concentration range of $12.5{\mu}g/ml$ to $200{\mu}g/ml$. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.04~1.23% and 0.08~0.68%, respectively, and the overall recoveries of 97.45~105.58% for the two compounds analyzed. Additionally, a difference was observed in the cluster analysis and principal component analysis between Cyperi Rhizoma in Korea and China. The result demonstrated that the principal component analysis is useful to distinguish between Cyperi Rhizoma in Korea and China.

• 대한화학회지
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• 제32권3호
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• pp.211-226
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• 1988

역상 액체 크로마토그래피에 의하여 몇 가지 금속-dithiocarbamate(DTC) 킬레이트의 용리거동을 Novapak $C_{18}$과 {\mu}$-Bondapak $C_{18}$ 분리관을 사용하여 연구하고, 아울러 동시 분리정량에 미치는 pH, 진탕시간, 흐름속도, 추출용매 종류 및 이동상의 세기등 여러가지 인자들의 영향을 조사 검토하였다. 미량 금속-DTC 킬레이트들은 Novapak $C_{18}$ 분리관에서 acetonitrile/methanol/water 또는 acetonitrile/water의 용리액을 사용하여 성공적으로 분리되었다. 모든 금속-DTC 킬레이트의 용매세기 인자는 $0{\leqq}log\;k'{\leqq}1$ 의 범위임을 확인하였고, 회수율을 97.0-106.7 %, coefficient of variation은 0.98-3.41%이었다. 최적 분석 조건에서 합성 시료중에 있는 혼합 금속 이온들은 상대 오차 ${\pm}$6.7 % 이내에서 동시 분리정량이 가능하였다.

• Bulletin of the Korean Chemical Society
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• 제33권2호
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• pp.559-563
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• 2012

An analytical method for the simultaneous determination of veterinary medicines (amprolium and decoquinate) in cattle and chicken's muscle by HPLC/UV-vis was established. Samples were extracted by a HLB (Hydrophilic-Liphophilic Balance) cartridge with acetonitrile and methanol. Prior to HPLC injection, a mixture solvent (Water:MeOH, 1:1) was utilized as a reconstitution solvent. Chromatographic separation was achieved with a C18 column ($250{\times}4.6mm$, $5{\mu}m$) using gradient elution with 20 mM HFBA and MeOH:ACN (1:1.8). The calibration curves from the spiked blank matrix showed good linearity (above $r^2$=0.997) in the concentration range of $0.13-12.0mg\;kg^{-1}$. The relative recovery (accuracy) and limit of quantitation (LOQ) were in the range of 78.5-107.1% and $0.13-0.42mg\;kg^{-1}$, respectively. The developed method can be used to determine under the MRL (Maximum Residue Limits) levels of veterinary medicines in animal tissues.

• 한국식품영양과학회지
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• 제3권1호
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• pp.69-76
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• 1974

The method of amino acid sequence determination from the C-terminal amino acid is proposed and mass spectrometric identification of thiohydantoins described previously. In this paper was discussed the fragmentation of thiohydantoin-ring by deutero substitution and model tripeptide have been degraded through three stages each, with interpretable results. The conditions employed in this method are mild enough for biological materials. The main features of the method are the following. 1. Thiohydantoins were formed in a non-aqueous medium a mixture of acetic anhydride, acetic acid and ammonium thiocyanate. 2. Mass sepectra of thiohydantoins derived from 20 amino acids were obtained with a mass spectrometer, JEOL model JMS-06H. 3. Cleavage of peptidyl thiohydantoin was made with an acidic from of a cation-exchange resin. (Amberlite IR-120) 4. Separation of the cleaved thiohydantoin and the parent peptide less one amino acid moiety was made by chromatography on a Sephadex G-10 column. 5. The peptide fraction was concentrated by freezedrying. 6. Thiohydantoin derivative of carboxyl terminal amino acid residue was introduced with a direct inlet probe in methanol solution.

• Toxicological Research
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• 제29권3호
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• pp.203-209
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• 2013

A simple and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantification of ${\varepsilon}$-acetamidocaproic acid (AACA), the primary metabolite of zinc acexamate (ZAC), in rat plasma by using normetanephrine as an internal standard. Sample preparation involved protein precipitation using methanol. Separation was achieved on a Gemini-NX $C_{18}$ column ($150mm{\times}2.0mm$, i.d., 3 ${\mu}m$ particle size) using a mixture of 0.1% formic acid-water : acetonitrile (80 : 20, v/v) as the mobile phase at a flow rate of 200 ${\mu}l/min$. Quantification was performed on a triple quadrupole mass spectrometer employing electrospray ionization and operating in multiple reaction monitoring (MRM) and positive ion mode. The total chromatographic run time was 4.0 min, and the calibration curves of AACA were linear over the concentration range of 20~5000 ng/ml in rat plasma. The coefficient of variation and relative error at four QC levels were ranged from 1.0% to 5.8% and from -8.4% to 6.6%, respectively. The present method was successfully applied for estimating the pharmacokinetic parameters of AACA following intravenous or oral administration of ZAC to rats.

• Natural Product Sciences
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• 제16권4호
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• pp.251-258
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• 2010

In this study, quantitative analysis for the quality evaluation of Salviae Miltiorrhizae Radix using HPLC/UV was developed. For quantitative analysis, six major bioactive compounds were determined. The separation conditions employed for HPLC/UV were optimized using ODS $C_{18}$ column ($250{\times}4.6\;mm$, $5\;{\mu}m$) with gradient condition of A (1% formic acid in $H_2O$) and B (acetonitrile : methanol : formic acid = 100 : 75 : 1) as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 280 nm. These methods were fully validated with respect to the linearity, accuracy, precision and recovery. The HPLC/UV method was applied successfully to the quantification of six major compounds in the Salviae Miltiorrhizae Radix. The results indicate that the established HPLC/UV method is suitable for the quantitative analysis.

• 생약학회지
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• 제45권4호
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• pp.294-299
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• 2014

The simultaneous determination of platyphylloside, aceroside and betulin was established for the quality control of Betula platyphylla bark using a high performance liquid chromatography and diode-array UV/Vis detector (HPLC-DAD). Separation and quantification were successfully achieved with a INNO C18 column ($5{\mu}m$, 4.6 mm $I.D.{\times}150mm$) by gradient elution of a mixture of methanol and water at a flow rate of 1.0 ml/min. Validation of the developed method was performed by various factor such as linearity, specificity, precision, accuracy, system suitability and stability. This method was successfully applied to the determination of contents of platyphylloside, aceroside VIII and betulin in three batches of Betula platyphylla bark extract. These results suggest that the developed HPLC method is simple, effective and could be utilized as a quality control method for Betula platyphylla bark products.

• Natural Product Sciences
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• 제17권4호
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• pp.321-327
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• 2011

In this study, quantitative analysis was developed using HPLC/UVD for the quality evaluation of Scutellariae Radix. For quantitative analysis, six major bioactive compounds were assessed. The separation conditions employed for HPLC/UVD were optimized using Phenomenex $C_{18}$ column ($250{\times}4.6$ mm, 5 ${\mu}m$) with a gradient of solvent A (1% acetic acid of $H_2O$) and solvent B (acetonitrile : methanol : acetic acid = 70 : 30 : 1) as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 275 nm. These methods were fully validated with respect to linearity, accuracy, precision and recovery. The HPLC/UVD method was applied successfully to the quantification of six major compounds in the extract of Scutellariae Radix. The results indicate that the established HPLC/UVD method is suitable for the quantitative analysis and quality control of multicomponents in Scutellariae Radix.

• 대한화학회지
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• 제30권3호
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• pp.312-319
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• 1986

알킬 처리된 실리카(ODS)칼럼을 정지상으로하여 역상에서의 이온-쌍 크로마토그래피 법으로 방향족 카르복시산들의 크기 인자를 조사하고 분리하는데 반대 이온으로 브롬화 도데실트리메틸암모늄(DTAB)을 사용하였다. 시료의 크기 인자는 반대 이온의 농도, 메탄올의 농도, 전해질의 종류 및 농도, 시료 분자에 붙어 있는 다른 작용기의 종류 및 위치등에 따라 영향을 받았다. 최적 조건하에서 몇 가지 혼합 시료를 분리할 수 있었다.