• Journal of Ginseng Research
• /
• 제32권4호
• /
• pp.390-396
• /
• 2008

For evaluating the quality of ginseng, simple and fast analysis methods are needed to determine the ginsenoside content of the ginseng products. The aim of this study was therefore to optimize conditions for fast analysis of the ginsenosides, the active ingredients in extracts of Korean red ginseng. When tandem HPLC mass spectrometry (HPLC-MS/MS) was used, four forms of ginsenoside, Rb1, Rb2, Rc, and Re, were readily separated in seven minutes using a gradient mobile phase (acetonitrile and water containing acetic acid). This is the shortest separation time reported among the studies of major ginsenoside analysis. When gradient HPLC with UV detection was used, the detection limit was high, but separation of these four ginsenosides required 25 minutes using acetonitrile and water containing formic acid as a mobile phase. HPLC-MS/MS was able to separate ginsenoside Rg1 easily regardless of the mobile phase condition, but the HPLC-UV could not separate Rg1 because acetonitrile concentration in the mobile phase had to be maintained below 20%. Ginsenoside peaks were clearer and had more sensitive detection limits when Korean red ginseng extract was analyzed by the HPLC-MS/MS, but the UV detection was useful for chromatographic fingerprinting of all four major ginsenosides of the extract: Rb1, Rb2, Rc, and Re. Extracts were found to contain 2.17 mg, 1.51 mg, 1.29 mg, and 0.46 mg of ginsenoside Rb1, Rb2, Rc, Re, respectively, per gram weight. The ratios of each ginsenoside in the extracts were 1.0 : 0.7 : 0.6 : 0.2, respectively. Taken together, the results indicate that HPLC-MS/MS spectrometry could be the most useful method for rapid analysis of even small amounts of major ginsenosides, while HPLC with UV detection could also be used for rapid analysis of major ginsenosides and for quality control of ginseng products.

• 분석과학
• /
• 제26권1호
• /
• pp.19-26
• /
• 2013

자외선 흡광도가 거의 없는 농작물의 생장 조절용 농약으로 사용되고 있는 지베렐린(GAs) 중 하나인 지베렐린 산($GA_3$)은 발색단이 미약해서 자외선 검출기를 이용하여 분석하기가 어려운 물질이다. 액체-액체 추출법을 이용하여 과일류로부터 지베렐린 산을 효과적으로 추출하기 위하여 시료의 pH와 추출용매에 대한 최적의 추출조건을 확립하고자 하였다. 페나실 브로마이드를 유도체화 시약으로 사용함으로써 자외선 검출기에 선택적이며 감도가 좋은 $GA_3$-유도체 화합물을 만들었으며, 최적의 유도체화 조건을 확립하기 위해서 반응온도 및 시간, 유도체화 시약의 양, 염기의 양 등을 변화시켜주는 실험이 수행되었다. 유도체화 된 $GA_3$는 C18 컬럼을 사용하여 방해물질이 없이 HPLC/UV-vis로 효과적으로 분석되었으며, HPLC/ESI-MS를 사용하여 유도체화된 화합물의 구조를 확인하였다. 사과의 경우, 검출한계(LOD)와 정량한계(LOQ)는 각각 0.008 mg/kg, 0.027 mg/kg로, 배의 경우, 검출한계(LOD)와 정량한계(LOQ)는 각각 0.003 mg/kg, 0.012 mg/kg로 낮은 검출한계와 정량한계를 보였다. 확립된 유도체화 방법은 과일류 중에 존재하는 $GA_3$의 효과적이고 편리한 분석에 응용될 수 있을 것이다.

• 분석과학
• /
• 제30권2호
• /
• pp.82-88
• /
• 2017

Adenophorae Radix (AR) is a frequently used medicinal herb; because of its popularity, products containing similar herbal products are often sold as substitutes, especially if their morphology is similar. However, any analytical method to identify AR based on quantitative analysis is not registered in Korea, Japan and China Pharmacopoeias. This study developed a simple HPLC method to discriminate between authentic AR and substitutes. Linoleic acid was used as a marker compound of AR. Our optimized HPLC-UV conditions included a mobile phase of 90 % acetonitrile under isocratic condition, and a flow rate of 1.0 mL/min at room temperature. Detection wavelength was set at 205 nm. Linoleic acid was detected at 13.5 minutes for a total analysis time of 20 minutes. The standard herb of AR contained 0.025 % of linoleic acid, while four authentic AR samples and eight substitutes contained 0.040~0.071 % and 0.004~0.014 %, respectively. Comparison of the linoleic acid concentrations of the sample types to reference AR showed that among 12 samples, only the four samples were authentic. Thus, our HPLC-UV method, along with our suggested content criterion for linoleic acid concentration, can be used for the quick and accurate determination whether the herbal products are authentic AR or substitute.

• 생약학회지
• /
• 제43권4호
• /
• pp.286-290
• /
• 2012

Many diterpenoids from Siegesbeckia species (Compositae) and their anti-inflammatory actions have been examined. In this research, high-performance liquid chromatography-ultraviolet spectrophotometer (HPLC-UV) method was used to compare the quantitative level of kirenol (ent-pimarane-type diterpenoid) in the aerial parts of Korean S. glabrescens and S. pubescens and the Chinese Siegesbeckiae Herba. Fingerprints of the two HPLC chromatograms of Korean S. glabrescens and S. pubescens were similar, but considerably different from Chinese Siegesbeckiae Herba. The content of kirenol in S. pubescens ($16.51{\pm}0.10$ mg/ml dry weight as mean${\pm}$RSD) was higher than S. glabrescens ($13.48{\pm}0.12$ mg/g dry weight). These values were considerably higher than the Chinese Siegesbeckiae Herba ($1.55{\pm}0.74$ mg/g dry weight). Thin layer chromatography (TLC) analysis demonstrated the containing of kirenol in the three plant materials, but the presence of siegeskaurolic acid (entkaurane-type diterpenoid) only in the Chinese Siegesbeckiae Herba.

• 분석과학
• /
• 제6권4호
• /
• pp.411-415
• /
• 1993

지방산을 UV 검출기를 사용하여 HPLC로 분석하기 위하여 2-bromoacetyltriphenylene을 유도체화제로 응용하였다. 18-crown-6-ether를 촉매로 한 유도체화반응은 매우 신속, 간편하고 정량적으로 진행되었으며, HPLC상에서 지방산의 검출한계가 1ng 수준으로 그 감도가 양호하였다. 또한 $C_{12}$부터 $C_{22}$까지 9종류의 포화지방산이 역상컬럼상에서 acetonitrile-물 gradient 조건으로 동시에 분리가 가능하였다. 이를 응용하면 각종 생체 시료로부터 미량의 지방산들에 대한 동시분석이 가능하리라 기대된다.

• 한국식품저장유통학회지
• /
• 제24권6호
• /
• pp.795-801
• /
• 2017

개별인정형 건강기능식품 기능성 원료로 개발한 두릅추출물의 표준화를 위해 항고혈압활성 효과를 가지고 있는 기능성분 HE를 지표성분으로 설정하고, HPLC/UV 방법을 이용하여 기능성분 분석법을 확립하며 그에 따른 유효성 검증을 실시하고자 하였다. 유효성 검증 결과, 본 시험법에서 표준용액의 피크유지시간과 두릅추출물의 피크유지시간이 일치하였다. 검량선의 결정 계수(R2)는 0.9999 이상의 높은 직선성을 보여 분석에 적합함을 알 수 있었으며, 검출 한계는 $12.0{\mu}g/mL$, 정량한계는 $36.5{\mu}g/mL$로 두릅 추출물 중의 HE 함량분석을 위한 충분한 한계 수준으로 확인되었다. 정확성에서 $98.8{\pm}0.865-104.7{\pm}2.536%$로 높은 수준의 HE 회수율을 보였으며, 평균 분석오차는 0.013%로서 기준인 10% 이내를 만족하였다. 또한 반복성에서는 평균 $101.5{\pm}0.4%$로 RSD 0.4%를 나타내었고, 실험실내 정밀성에서 RSD 0.2%, 완건성에서 RSD 0.2%를 나타내어 모두 적합함을 확인하였다. 한편, 제주산 두릅추출물 중에는 기능성 지표성분인 HE가 4.88% 함유되어 있는 것으로 확인되었다. 이상의 실험 결과, 두릅추출물의 항고혈압활성 기능성분인 HE의 HPLC/UV 분석방법은 특이성, 직선성, 정확성, 정밀성, 반복성, 완건성 등의 모든 항목에서 validation 기준에 적합한 시험 방법으로 확인되었다.

• 한국한의학연구원논문집
• /
• 제1권1호
• /
• pp.441-459
• /
• 1995

To study stability of distilled herbal medicine, we chose changes in UV spectrum, pH, conductivity, and HPLC chromatogram. Aconiti Lateralis preparata Radix and Scutellariae Radix were selected and studied. There ws no consistancy in UV spectrums of preparatons and in duration. The changes in pH and conductivity were not correlated to those in UV spectrums. HPLC chromatograms were also compared each other depending on the preparations. One interesting peak of distilled Aconiti solution was appeared at 40 min retention time which was not identified yet. Ingeneral, UV spectrum, pH, conductivity measurements are pretty poor tool to study stability of herbal medicine although HPLC analysis should be studied further.

• Journal of Applied Biological Chemistry
• /
• 제64권1호
• /
• pp.63-67
• /
• 2021

Isovitexin, a marker compound with various pharmacological activities, in Lespedeza cuneata, was analyzed using high performance liquid chromatography coupled with UV (HPLC/UV). There are no previous reports on using L. cuneata as the source material for the quantification of isovitexin. In this study, we developed an optimized method using HPLC-UV analysis, which was validated using various parameters. Our method demonstrated high specificity, and good separation of the chromatographic peak was achieved. Parameters such as linearity (r2≥0.9997), precision, and accuracy indicated that our proposed analytical method had good reliability and sensitivity. These results demonstrate the utility and convenience of our method for rapidly quantifying isovitexin in L. cuneata extracts.

• 대한본초학회지
• /
• 제23권1호
• /
• pp.109-116
• /
• 2008

Objectives : This study was performed to investigate the discriminative criteria of 6 kinds of Achyranthis Radix by HPLC/DAD. Methods : 20-hydroxyecdysone is isolated by silica gel column chromatography ($CHCl_3$:MeOH, 7:1-1:1 v/v) and identified by nuclear magnetic resonance, A high-performance liquid chromatographic method with diode array detection was used to identify 20-hydroxyecdysone in A. japonica. The analysis was performed using $C_{18}$ column with isocratic elution consisted of 18% acetonitrile and 82% water and the detection was carried out by DAD at 254 nm. 6 kinds of Achyranthis Radix from different locations were extracted in MeOH. Each extracts was analyzed by HPLC in same condition as used in analysis of 20-hydroxyecdysone. The identities of each extracts were determined by comparing the retention time and UV spectrum with that of reference compound. Results : 1. A. japonica and A. bidentata showed the similar patterns of HPLC chromatogram and 20-hydroxycedysone was present in both of them because the peaks having the same retention time and UV spectrum as 20-hydroxyecdysone were shown in the HPLC chromatograms of A. japonica and A. bidentata 2. Cyathula officinalis and C. capitata showed the similar patterns of HPLC chromatogram. The peak having the same retention time and UV spectrum as 20-hydroxyecdysone was shown in the HPLC chromatogram of C. capitata but not shown in the HPLC chromatogram of C. officinalis. 3. Two species of medicinal drugs from Sacheon province showed similar patterns of HPLC chromatogram. Achyranthis Radix from Sacheon(wild) did not have 20-hydroxycedysone but Achyranthis Radix from Sacheon(cultivated) showed the peak having the same retention time as 20-hydroxyecdysone but UV spectrum of the peak was different from that of 20-hydroxyecdysone. Conclusions : These results suggested that 20-hydroxyecdysone could be the discriminative criteria for Achyranthis Radix contain 20-hydroxyecdysone though they belong to different genus and species. And the patterns of HPLC chromatogram also could be the discriminative criteria as the different species of Achyranthis Radix belonging to the same genus showed similar patterns of HPLC chromatogram.

• Bulletin of the Korean Chemical Society
• /
• 제35권3호
• /
• pp.765-769
• /
• 2014

An analytical methodology was developed for qualitative and quantitative impurity profiling of the coloring agent Sudan III by high-performance liquid chromatography (HPLC)-diode array detection (DAD). The impurities in commercial Sudan III were characterized by comparison of their retention times and UV spectra with those of authentic standards. Four impurities regulated by International Committees in Sudan III were quantified by HPLC-selective UV detection. The impurities in Sudan dye were successfully separated on a reversed phase C18-column within 25 min and sensitively detected by UV spectrometry at two selective wavelengths. Method validation was conducted to determine linearity, precision, accuracy, and limit of quantification (LOQ). The linear dynamic range extended from 0.002 to 4.0%, with a correlation coefficient (R2) greater than 0.995. The LOQs of the impurities ranged from 8.04 to $54.29{\mu}g/mg$. Based on the established method, the levels of regulated impurities in five commercial Sudan III dyes were determined.