• Natural Product Sciences
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• 제28권4호
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• pp.168-180
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• 2022

Ephedra is a genus of the Ephedraceae family and is found in temperate regions, such as Central Asia and Europe. Among the various ephedra species, Ma Huang (Ephedra herb) is derived from the aerial parts of Ephedra sinica S tapf, Ephedra equisetina Bunge, and Ephedra intermedia Schrenk & C.A. Mey. Ma Huang contains various ephedra alkaloids, including (-)-ephedrine, (+)-pseudoephedrine, (-)-norephedrine, (+)-norpseudoephedrine, (-)-methylephedrine, and (+)-methylpseudoephedrine, which are found naturally as single enantiomers, although they can be prepared as racemates. Although the use of Ma Huang in foods is prohibited in Korea, products containing Ma Huang can be imported, and so it is necessary to develop a suitable analytical technique for the detection of Ma Huang in foods. Herein, we report the development of analytical methods for the detection of ephedra alkaloids in products containing Ma Huang. Following sample purification by solid phase extraction, quantitative analysis was performed using ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). Additionally, the enantiomers were successfully separated using HPLC-DAD. We successfully analyzed various food samples, where the ephedra alkaloids were qualitatively and quantitatively determined, and the enantiomers were separated. It is expected that these methods may contribute toward preventing the distribution of illegal products containing Ma Huang.

• Natural Product Sciences
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• 제12권1호
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• pp.55-61
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• 2006

A description of simple, isocratic and precise reversed phase HPLC methods is given for simultaneous quantification of pholcodine and ephedrine hydrochloride together with either carbinoxamine maleate or terfenadine in antitussive-antihistaminic oral pharmaceutical formulations. Separations were carried out on X-Terra and symmetry shield C18 column $(250\;{\times}\;4.6\;mm,\;5\;{\mu}m)$. The used isocratic elution systems were either $0.02\;M\;KH_2PO_4-acetonitrile$ in the ratio of 75 : 25 and pH adjusted to 7.70 with orthophosphoric acid or sodium hydroxide, for syrup (method A), or 0.02 octanesulphonic acid sodium salt solution-acetonitrile-acetic acid in the ratio of 75 : 25 : 0.5 for suspension (method B). The elution of both mixtures was achieved with a flow rate of 1 ml/min. Detection was carried out by UV absorbance at wavelengths of 220 and 250 nm for syrup and suspension, respectively. The quantification of the components in synthetic mixtures and actual syrup and suspension were calculated using the internal standard technique with metoclopramide HCl and codeine phosphate as internal standards (IS), respectively. The methods, for both mixtures, were validated and met all the requirements for the quality control analysis recommended by FDA and ICH.

• 대한본초학회지
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• 제20권4호
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• pp.133-140
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• 2005

Objectives : We have been used many herbal medicines after processing to improve the effect, decrease toxicity and side-effect, and change property. We have studied the physico-chemical change and HPLC pattern of Morindae Radix by means of processing method. Methods : This study was investigated the contents of loss on drying, residue on ignition, residue on acid insoluble ignition, 50% ethanol extract and HPLC pattern of Morindae Radix(Morinda officinalis How.) by processed and non-processed. We have conducted Morindae Radix and Damnacanthi Radix which is circulated in herbal medicine market by forgery. Processed Morindae Radix was prepared by heating of added to salt(SP), liquor(LP) and Glycyrrhizae Radix solution(GP) for 20-40 minutes. Results and Conclusions : From this analysis, we found that the content of 50% ethanol extract was increased by processing method. And we were detected distinguishable marker of processed and non-processed from Morindae Radix(Morinda officinalis How.) by HPLC pattern analysis.

• 한국동물위생학회지
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• 제26권3호
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• pp.199-202
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• 2003

Solid phase extraction(SPE) and matrix solid phase dispersion(MSPD) have been studied as preparation procedures for tetracyclines analysis by high-performance liquid chromatography(HPLC) in meat. The recovery range was 74${\sim}$98% for SPE, and 72${\sim}$93% for MSPD at spiked levels of 100ng/g for oxytetracycline(OTC), tetracycline(TC), chlortetracycline(CTC), and doxycycline(DC). The detection limits were 15${\sim}$78ng/g for SPE and 25${\sim}$84ng/g for MSPD, respectively. Analytical method was HPLC with UV detector. The purpose of this study was developing a practical, accurate and precise method for rapid extraction and quantitation of tetracycline residues in meat.

• 약학회지
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• 제44권2호
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• pp.135-140
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• 2000

Determination of Aconitum alkaloids in processed Buza (Cho-0, Salted Buza, Moist-heating Buza, Limed Buza), which had been prepared from the raw tubers of Aconitum chiisanenseb(Ranunculaceae), was established using visible spectrophotometry and high-performance liquid chromatography (HPLC) method especially for Aconitine analysis. Aconitum alkloids were reacted with tetra- thiocy-anatocobalt[II] complex ion to form a stable ion pair. The reaction product was insoluble in water but freely soluble in several organic solvents. 1.2-Dichloroethane was the best extracting solvent among the examined solvents. Spectrophotometry of Aconitum alkaloids at nax. 625 was carried out. The HPLC method for aconitine was carried out using Radial PAK-CN column with gradient solvent system by solvent mixture of acetonitrile and phosphate buffer (pH 3.0) at 4$0^{\circ}C$ and 254 nm. Linear relationship was found between absorbance response and concentration of aconitine in range of 0.45 mM~0.9 mM ($r^2$=0.9949) by spectrophotometry and 0.3 mM~1.2mM($r^2$=0.9983) by HPLC method. These methods have been found to be suitable and reproducible for routine analysis of Aconitum alkaloids and its pharmaceutical preparations.

• 한국연초학회지
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• 제2권2호
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• pp.1-7
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• 1980

오리엔트산 및 한국산 향끽미종 잎담배의 휘발성이 적은 성분들을 간단한 장치와 간단한 조작을 통해 분리 농축하였다. 각 휘발성이 적은 농축물들은 가시 영역에서 흡광도를 측정하고 박층 크로마토그라피 (TLC)와 고성능 액체 크로마토그라피 (HPLC)에 의해서 상세한 조성분석을 하였다. 각 품종간의 정량적인 차이가 가시광선 흡수 스펙트라, TLC 패턴, HPLC프로파일 상에서 확인되었다.

• 분석과학
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• 제36권1호
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• pp.22-31
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• 2023

As the use of e-liquid cigarettes is rapidly increasing worldwide, it multiplies the potential risk undisclosed to the health of non- and smokers. To reduce the hazard, each country has its own set of regulations for controlling e-liquids. In Korea, the narrow definition of tobacco makes it difficult and have been steadily occurring tax evasion exploiting the difference in natural and artificial nicotine. Therefore, it is very important to distinguish source of nicotine for their regulation. To find biochemical discriminant markers, this study established analysis methods based on high-performance liquid chromatography coupled with diode array detector (HPLC-DAD) and high-performance liquid chromatography coupled with triple Quadrupole mass spectrometry (HPLC-MS/MS) for nicotine enantiomers and tobacco alkaloids targeted using the difference in pathways of nicotine biosynthesis and chemical synthesis. The method was validated by experimenting linearity (R² > 0.999), recovery (80.99-108.41 %), accuracy (94.11-109.73 %) and precision (0.04-8.27 %). Then, the results for discrimination of the nicotine obtained from analysis of 65 commercial e-liquid products available in Korean market was evaluated. The method successfully applied to the e-liquids and one sample labelled 'synthetic nicotine' for tax exemption was found to contain a natural nicotine product. This method can be used to determine whether an e-liquid product uses natural or artificial nicotine and monitor non-taxable e-liquid products. The method is more scientific than the existing one, which relies only on field evidence.

• 한국연초학회지
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• 제28권2호
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• pp.130-135
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• 2006

This study was carried out to improve the analytical methods for determination of organic acids in tobacco leaf by HPLC. The samples for HPLC analysis were pre-treated by means of SPE. The calibration curve for each acid was linear and $R^2$ values ranged from 0.9990 to 1.0000. The limit of detection were obtained from the calibration curves and their values were between 1.39 to $4.87{\mu}g/mL$. Recovery rates of organic acids were between 88.6 % to 98.5 %. The concentrations of organic acids among the various tobacco leaves were compared to the concentration of organic acids, were in the order oriental, burley, flue-cured tobacco. In the case of flue-cured and oriental tobacco leaves, the order of concentration of organic acids was malic acid, oxalic acid, citric acid. But in the case of burley tobacco leaves, the order of concentration of organic acids was citric acid, oxalic acid, malic acid.

• 생약학회지
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• 제48권1호
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• pp.77-81
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• 2017

The aim of this study was to investigate a validation method for determination of tricin in Phragmites communis ears. Tricin was isolated with chromatographic methods and used as the standard substances for quantitative analysis. The structural determination was characterized by comparing their NMR spectral data with values reported in the literature. For validation, the specificity, linearity, precision, accuracy, detection limits, and quantification limits of tricin was measured by HPLC. The results show that the specificity was satisfied with retention time and diode array detector (DAD) spectrum by analysis of tricin using HPLC. The limits of detection (LOD) for tricin was 0.84 mg/ml. Recovery of tricin was 98.80~108.22% with R.S.D values less than 2%. Intra-day and inter-day precisions of tricin in P. communis ears were 99.96~100.96% and 99.01~100.40%, respectively. Therefore, application of tricin was validated by an analytical method as major compound in P. communis ears.

• 한국환경농학회지
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• 제34권3호
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• pp.196-203
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• 2015

BACKGROUND: Purpose of this research is HPLC analysis method development of lycopene in tomato. And then, three components of carotenoid in four kinds of tomatoes (general tomato, cherry tomato, red and orange date tomato) were compared with each other. METHODS AND RESULTS: Lycopene in tomato was extracted with hexane likes other carotenoid components using 500 mg of dried powder sample. HPLC analysis conditions were column temperature ($40^{\circ}C$), detection wavelength (454 nm), flow rate (1.0 mL/min) and injection volume ($20.0{\mu}L$). Lycopene was analyzed by the gradient elution ($60{\rightarrow}100%$) of the mobile phase solvents A[water: methanol=25: 75 (v/v)] and B[ethyl acetate]. CONCLUSION: Three components of carotenoids (lutein, ${\beta}$-carotene, lycopene) were observed in tomatoes. The total carotenoid contents was the highest in red date tomato (662.0 mg/kg dry wt.) and the lowest in orange date tomato (111.3 mg/kg dry wt.). Lycopene contents in tomatoes was the highest percentage (93%) among all the carotenoids.