• Journal of Ginseng Research
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• 제40권4호
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• pp.382-394
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• 2016

Background: Ginsenosides are the characteristic and principal components which manifest a variety of the biological and pharmacological activities of the roots and rhizomes of Panax ginseng (GRR). This study was carried out to qualitatively and quantitatively determine the ginsenosides in the cultivated and forest GRR. Methods: A rapid and sensitive ultra-high-performance liquid chromatography coupled with diode-array detector and quadrupole/time of flight tandem mass spectrometry (UPLC-DAD-QTOF-MS/MS) was applied to the qualitative analysis of ginsenosides and a 4000 QTRAP triple quadrupole tandem mass spectrometer (HPLC-ESI-MS) was applied to quantitative analysis of 19 ginsenosides. Results: In the qualitative analysis, all ingredients were separated in 10 min. A total of 131 ginsenosides were detected in cultivated and forest GRR. The method for the quantitative determination was validated for linearity, precision, and limits of detection and quantification. 19 representative ginsenosides were quantitated. The total content of all 19 ginsenosides in the forest GRR were much higher than those in the cultivated GRR, and were increased with the growing ages. Conclusion: This newly developed analysis method could be applied to the quality assessment of GRR as well as the distinction between cultivated and forest GRR.

• Natural Product Sciences
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• 제16권2호
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• pp.116-122
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• 2010

A high-performance liquid chromatography (HPLC) with diode array detector (DAD) and electrospray ionization mass spectrometry (ESI-MS) was established for the simultaneous determination of five representative metabolites of the iridoid and phenolic classes from Rehmannia glutinosa. The optimal chromatographic conditions were obtained on an ODS column (5 mm, $4.6{\times}250\;mm$) with the column temperature at $25^{\circ}C$. The mobile phase was composed of water and acetonitrile using a gradient elution with the flow rate 0.3 mL/min. Detection wavelength was set at 205 nm. All calibration curves showed good linear regression ($r^2$ > 0.997) within test ranges. Limits of detection (LOD) and quantitation (LOQ) values were lower than 0.123 and $0.373\;{\mu}g/mL$, respectively. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.09 - 0.76% and 0.16 - 1.41%, respectively, and the overall recoveries of 99.03 - 102.67% for all of the compounds analyzed. In addition, effectiveness of diverse extraction methods was compared to each other for the development of standard analytic method. The verified method was successfully applied to the quantitative determination of five representative metabolites in twenty-one commercial Rehmannia glutinosa samples from different markets in Korea and China. The analytical results showed that the contents of the five analytes vary significantly with sources.

• 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.

• 분석과학
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• 제26권1호
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• pp.1-10
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• 2013

많은 양봉업자들이 그들의 벌을 보호하기 위해 동물성의약품들을 사용한다. 우리나라에서 벌에 사용되는 동물성 의약품은 아미트라즈, 브로모프로필레이트, 쿠마포스, 시미아졸 등이다. 2006년 중반에 한국 정부에서는 아미트라즈와 쿠마포스의 최대잔류허용기준을 각각 0.2, 0.1 ppm으로 설정하였다. 해마다 양봉환경이 변하고 있으므로 꿀 속의 동물성 의약품들에 대한 지속적인 모니터링이 필요하다. 본 연구에서는 2011년에 지역시장이나 인터넷을 통해 모은 10개 벌꿀 시료들에 대하여 아미트라즈, 브로모프로필레이트, 쿠마포스, 시미아졸 잔존량을 HPLC-DAD로 조사하였다. 조사한 10종의 벌꿀에서는 살충제로 사용되는 이들 성분이 25 ppb 이상으로는 검출되지 않았다.

• 약학회지
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• 제57권3호
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• pp.167-172
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• 2013

Insampaedoksan (IS) is the decoction of medicinal herbs, which was commonly used for anti-inflammatory and anti-pyretic in the Korean traditional medicine (KTM). Several studies on improving efficiency or searching new efficiency by fermenting traditional herbal medicines are recently in progress. The bioconversion has been conducted on IS using various bacteria. Liquiritin, ferulic acid, hesperidin, liquiritigenin, and glycyrrhizin in IS before and after fermented IS were simultaneously analyzed. These compounds were qualitatively analyzed and quantitatively analyzed using the HPLC-DAD system. The identifications of liquiritin, ferulic acid, hesperidin, liquiritigenin and glycyrrhizin were achieved by comparing the HPLC retention time ($R_t$) and the UV absorption of five pure compounds in the IS. As a result, the increased constituents were identified to be liquiritin, liquiritigenin and glycyrrhizin, while the decreased constituent was ferulic acid and the constituent of hesperidin was similar to before and after fermentation. Insampeadock-san fermented by Lactobacillus plantarum KFRI 144 exhibited the most remarkable changes in all of fermentation.

• 한국식품영양과학회지
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• 제37권1호
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• pp.124-128
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• 2008

본 연구는 DAD/UV HPLC를 이용하여 뽕잎과 오디(Morus alba L.)에 함유되어 있는 stilbenoids의 조성과 함량을 분석하고자 수행되었다. 뽕잎과 오디추출물을 DAD를 이용하여 최대흡광파장을 탐색한 결과 308 nm로 나타났으며, stilbenoids 조성이 오디에는 resveratrol, piceatannol, rhapontigenin, astringin, pterostilbene, piceid, rhaponticin, 뽕잎에는 resveratrol, rhapontigenin, pterostilbene, piceid이 함유된 것으로 나타났다. 오디와 뽕잎의 총 stilbenoids 함량은 $609.15{\pm}7.24$ mg/100 g d.w.와 $188.57{\pm}1.70$ mg/100 g d.w.였으며, rhaponticin은 오디($389.26{\pm}5.22$ mg/100 g d.w.)와 뽕잎($99.17{\pm}2.79$ mg/100 g d.w.) 모두 가장 많은 함량이 함유되어 있었다. Astringin과 piceatannol은 오디에서만 검출되었으며 vitisin A는 모두 검출되지 않았다. Piceid와 rhaponticin은 이의 비배당체인 resveratrol과 rhapontigenin보다 과량 함유되어 있어 비배당체보다는 배당체의 함량이 높은 것으로 나타났다.

• 약학회지
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• 제52권1호
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• pp.7-11
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• 2008

A high performance liquid chromatographic (HPLC) method for the determination of glycyrrhizic acid was developed for the quality control of traditional herbal medicinal preparation Bu-Zhong-Yi-Qi-Tang (BZYQT), which is well-known herbal medicine used as tonic. RP-HPLC analysis was carried out using Capcell pak $C_{18}$ MG column $(5\;{\mu},\;150{\times}4.6\;mm)$ and a mobile phase consisting of acetonitrile and water containing 0.03% phosphoric acid (pH 2.46) at a flow rate of 1.0 ml/min. The optimum wavelength for the detection of the glycyrrhizic acid was found at 250 nm using diode-array UV/VIS detector. The glycyrrhizic acid in BZYQT shows good linearity $(r^2>0.999)$ in the range of $15\;{\mu}g/ml$ to 500 ${\mu}g/ml$. The limit of detection (LOD) was less than 5 ng and R.S.D for intra-day and inter-day reproducibility was less than 7%. The mean recovery of the glycyrrhizic acid was $97.3{\sim}113.0%$. These results suggest that the developed HPLC method is simple and efficient, and could be contributed for the quality control of commercial BZYQT products.

• Journal of Acupuncture Research
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• 제32권2호
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• pp.1-9
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• 2015

Objectives : The present study was an evaluation and standardization of herbal components in order to establish the efficacy and safety of Shinbaro pharmacopuncture. Methods : Among the raw materials of Shinbaro pharmacopuncture, the components Cibotii Rhizoma, Eucommiae Cortex, and Ledebouriellae Radix were assessed through ingredient verification experiments using thin-layer chromatography(TLC) and ultraviolet rays(UV) lamps. In addition, we standardized Acanthopanacis Cortex and Achyranthis Radix through validation using high performance liquid chromatograph-diode array detector(HPLC-DAD). Results : As result appeared a blue-white fluorescence under ultraviolet rays; changed to dark green after adding 1 % ferric chloride solution(due to Cibotii Rhizoma), and presented a yellow-green fluorescence when mixed with an ethyl ether under UV lamps by way of the ethyl ether layer, confirming Eucommiae Cortex. Ledebouriellae Radix was confirmed as dark brown spots at Rf values of 0.56 and 0.71 using TLC. Additionally, Acanthopanacis Cortex and Achyranthis Radix HPLC test results showed that linearity was $R^2{\geq}0.99$, and detection limit and quantitation limit were 0.23 to $1.29{\mu}g/mL$, and 0.71 to $3.90{\mu}g/mL$, respectively. Furthermore, precision and accuracy were confirmed to have relative standard deviation(RSD) values of 0.10 to 1.89 % and 96.19 to 103.72 %, respectively. Shinbaro pharmacopuncture did not have any overlapping or interference from other peaks in detection under the abovementioned analysis conditions. Conclusions : In conclusion, we confirmed that maintenance of Shinbaro pharmacopuncture validity was possible by means of quality control of Cibotii Rhizoma, Eucommiae Cortex, and Ledebouriellae Radix through ingredient identification and Acanthopanacis Cortex and Achyranthis Radix through high performance liquid chromatograph(HPLC) analysis. Further, we hope to contribute to the development strategy of herbal industry acupuncture.

• 생약학회지
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• 제39권3호
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• pp.199-202
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• 2008

A high performance liquid chromatographic (HPLC) method for the simultaneous determination of hesperidin and glycyrrhizin was established for the quality control of traditional herbal medicinal preparation, Pyungwi-san (PWS). Separation and quantification were successfully achieved with a Waters XTerra RP18 column ($5{\mu}m$, 4.6 mm I.D. ${\times}$ 150 mm) by gradient elution of a mixture of acetonitrile and water containing 0.03% phosphoric acid (pH 2.03) at a flow rate of 1.0 ml/min. The diode-array UV/vis detector (DAD) was used for the detection and the wavelength for quantification was set at 230 nm. The presence of hesperidin and glycyrrhizin in this extract was ascertained by retention time, spiking with each authentic standard and UV spectrum. All four compounds showed good linearity $(r^2>0.995)$ in a relatively wide concentration ranges. The R.S.D. for intra-day and inter-day precision was less than 7.0% and the limits of detection (LOD) were less than 60 ng. The mean recovery of each compound was 99.0-105.6% with R.S.D. values less than 4.0%. This method was successfully applied to the determination of contents of hesperidin and glycyrrhizin in three commercial products of PWS. These results suggest that the developed HPLC method is simple, effective and could be readily utilized as a quality control method for commercial PWS products.

• 한국식품위생안전성학회지
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• 제35권4호
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• pp.326-333
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• 2020

본 연구는 불법적으로 식품에 사용될 수 있는 부정물질 11종에 대한 안전관리 강화를 위해 정량 및 정성 분석이 가능한 HPLC-DAD와 LC-MS/MS를 검증하기 위해 수행되었다. 확립된 시험법은 AOAC 가이드라인에 따라 직선성, 정밀성, 정량한계 및 회수율 등을 통해 유효성을 확인하였다. 본 실험에서 정량한계를 포함하여 검량선을 작성하였고, 모두 0.99 이상의 직선성을 확인하였다. 또한 정확성은 LC (90.0-106%), LC-MS/MS (83.0-114%) 이고, 정밀도는10% 이하로 재현성이 우수하였다. 확립된 시험법은 식품 중 부정물질 안전관리 및 모니터링에 활용될 것으로 사료된다.