• Title/Summary/Keyword: DAD-IS

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Simultaneous Determination of the Flavonoids and Limonoids in Citrus junos Seed Shells Using a UPLC-DAD-ESI/MS

  • Jo, Ara;Shin, Ji hun;Song, Hwa young;Lee, Ye Eun;Jeong, Da Eun;Oh, Sung Hwa;Mun, Myung Jae;Lee, Mina
    • Natural Product Sciences
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    • v.26 no.1
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    • pp.64-70
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    • 2020
  • Citrus junos seeds (CS) have been traditionally used for the treatment of cancer and neuralgia. They are also used to manufacture edible oil and cosmetic perfume. A large amount of CS shells without oil (CSS) are discarded after the oil in CS is used as foods or herbal remedy. To efficiently utilize CSS as a by-products, it needs to be studied through chemical analysis. Therefore, we developed an ultra-performance liquid chromatography (UPLC)-diode array detection (DAD) method for simultaneous determination and quantitative analysis of five components (two flavonoids and threes limonoids) in CSS. A Waters Acquity UPLC HSS T3 column C18 (2.1 × 100 mm, 1.8 ㎛) was used for this separation. It was maintained at 40 ℃. The mobile phase used for the analysis was distilled water and acetonitrile with gradient elution. To identify the quantity of the five components, a mass spectrometer (MS) with an electrospray ionization (ESI) source was used. The regression equation showed great linearity, with correlation coefficient ≥ 0.9912. Limits of detection (LOD) and limits of quantification (LOQ) of the five compounds were 0.09 - 0.13 and 0.26 - 0.38 ㎍/mL, respectively. Recoveries of extraction ranged from 97.45% to 101.91%. Relative standard deviation (RSD) values of intra- and inter-day precision were 0.06 - 1.15% and 0.19 - 0.25%, respectively. This UPLC-DAD method can be validated to simultaneously analyze quantities of marker flavonoids and limonoids in CSS.

Acute Oral Toxicity Study of Standardized Gami-Honghwa-Tang (KH-19) in Rats and Beagle Dogs (HPLC로 표준화한 가미홍화탕(KH-19)의 랫드와 Beagle견에 대한 단회경구투여독성시험)

  • Yu Young-Beob;Sung Hyun Jea;Yoon Yoo-Sik
    • Toxicological Research
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    • v.21 no.1
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    • pp.63-70
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    • 2005
  • Gami-Honghwa-Tang (KH-19), a herbal prescription for reducing the side effect of radiotherapy, is composed of eight crude herbs such as Rehmanniae Radix Preparata, Angelicae Gigantis Radix, Cnidii Rhizoma, Paeoniae Radix, Corni Fructus, Moutan Cortex Radicis, Lycii Fructus, Carthami Flos, and Glycyrrhizae Radix. In this study, marker substances in KH-19 were analyzed by high performance liquid chromatography-diode array detector (HPLC-DAD) and safety evaluation of standardized KH-19 was evaluated by good laboratory practices (GLP) guideline of Korea Food and Drug Administration. HPLC-DAD was employed to determine the quantities and the qualities of several marker substances such as 5-hydroxymethyl-2-furaldehyde (5-HMF), paeonol, loganin, paeoniflorin, glycyrrhizin, and decursin in the KH-19. In acute oral toxicity study on rat, transient inhibition of body weight was shown, but change in general symptom was not detected. No dead animal was observed up to 5,000 mg/kg in both male and female animals. In acute oral toxicity study on Beagle dog, transient vomiting, diarrhea, anorexia, and body weight reduction were observed, However, no dead animal was observed up to 2,000 mg/kg in both male and female animals.

Quantitative and Qualitative Analysis of Alkaloids in Coptis chinensis (Coptidis Rhizoma) by LC-DAD and LC-ESI/MS

  • Yu, Young-Beob;Bae, Chang-Hyu
    • Korean Journal of Plant Resources
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    • v.30 no.6
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    • pp.693-698
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    • 2017
  • The quality control of natural products is principal key to guarantee the Good Manufacturing Practices (GMP) and Good Clinical Practices (GCP) for the functional food, pharmaceuticals and cosmeceuticals in the industry. In this study, we examined the quantitative analysis of berberine as marker substance of Coptidis Rhizoma by high performance liquid chromatography-photodiode array detector (HPLC-DAD). The HPLC method was validated and met all the requirements for the quality control analysis recommended by FDA and ICH. The berberine was separated on a Xterra $C_{18}$ column ($5{\mu}m$, $4.6{\times}250mm$) using mobile phase consisting of distilled water and acetonitrile with $KH_2PO_4$ (3.4 g) and $Na_2SO_4$ (1.7 g). Calibration curve of berberine has been estimated (y = 42293.47x-41589 with the correlation coefficient 0.9999). The amount of berberine was calculated as 4.25%. And berberastine, palmatine, columbamine, jatrorrhizine, epiberberine, berberine and coptisine in the Coptidis Rhizoma were identified by high performance liquid chromatography - electrospray ionization-mass spectrometer (HPLC-ESI-MS) method.

Analysis of Bioconversion Compositions from Fermented Bojungikki-tangs (발효보중익기탕들의 생물전환성분 분석)

  • Kim, Dong-Seon;Roh, Joo-Hwan;Cho, Chang-Won;Ma, Jin-Yeul
    • YAKHAK HOEJI
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    • v.55 no.5
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    • pp.361-366
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    • 2011
  • Traditional herbal medicinal preparation Bojungikki-tang (BJT) is well-known herbal medicine used as tonic. We fermented Bojungikki-tang using nine lactic acid bacteria strains and discovered two remarkably increased compositions from the fermented BJTs using HPLC/DAD analysis. HPLC/DAD-guided fractionation of the increased compositions followed by structure identification using NMR and MS identified liquiritigenin and isoliquiritigenin. These bioconversion compositions were quantitatively analyzed using HPLC-DAD. Liquiritigenin contents were highest in BJTs fermented with L. amylophilus (1.91 mg/g) and L. fermentum (1.89 mg/g), which were increased by 20-fold compared to BJT (0.09 mg/g). Isoliquiritigenin contents were highest in BJTs in fermented with L. plantarum (0.19 mg/g) and L. fermentum (0.19 mg/g), which were increased by 19-fold compared to BJT (0.01 mg/g).

Tall Building Database-assisted Design: a Review of NIST Research

  • Yeo, DongHun;Potra, Florian A.;Simiu, Emil
    • International Journal of High-Rise Buildings
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    • v.8 no.4
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    • pp.265-273
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    • 2019
  • The purpose of this review paper is to briefly describe main the features of novel procedures developed by the National of Standards and Technology (NIST) for the design of tall buildings. Topics considered in the paper include: the division of tasks between wind and structural engineers; the determination of wind effects with specified mean recurrence intervals by accounting for wind directionality; the risk-consistent design of structures subjected to multiple wind hazards; iterative dynamic analyses and member sizing, including the use of modern optimization approaches; and commonalities of and differences between Database-assisted Design (DAD) and Equivalent Static Wind Loads procedures. An example of the application of the DAD procedure is presented for a reinforced concrete structure. Also included in the paper is an introduction to ongoing research on the estimation of wind load factors or of augmented design mean recurrence intervals commensurate with the uncertainties in the factors that determine the wind effects.

Quantitative Analysis and Enantiomeric Separation of Ephedra Alkaloids in Ma Huang Related Products by HPLC-DAD and UPLC-MS/MS

  • Kyoung-Moon Han;Jinwoo Hwang;Sun Hee Lee;Boreum Park;Hyungil Kim;Sun Young Baek
    • Natural Product Sciences
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    • v.28 no.4
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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.

Comparison of deck-anchored damper and clipped tuned mass damper on cable vibration reduction

  • Wu, W.J.;Cai, C.S.
    • Structural Engineering and Mechanics
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    • v.32 no.6
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    • pp.741-754
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    • 2009
  • Excessive cable vibrations are detrimental to cable-stayed bridges. Increasing the system damping of cables is a key solution to resolve this severe problem. Equations representing the dynamic characteristics of an inclined cable with a Deck-Anchored Damper (DAD) or with a Clipped Tuned Mass Dampers (CTMD) are reviewed. A theoretical comparison on the performance of cable vibration reduction between the cable-DAD system and the cable-CTMD systems is thoroughly discussed. Optimal system modal damping for the free vibration and transfer functions for the forced vibration for the two cabledamper systems are addressed and compared in detail. Design examples for these two different dampers are also provided.

Oxidation of Alkane Derivatives by Corynebacterium sp. (Alkane 유도체의 미생물학적 산화 제1보)

  • 이종근;이상준
    • Korean Journal of Microbiology
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    • v.21 no.4
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    • pp.185-190
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    • 1983
  • Twelve Microorganisms capable of utilizing diaminododecane were isolated from the soil by enrichment culture technique. Seven strains of these were identified as Corynebacterium. The isolated strains were tested for the ability to utilize as carbon source, 10 different kind of alkane derivatives containing CN, $NH_2$, Cl, and SH groups. Laurylcyanide, dicyanooetane, chlorodecane, and dichlorodecane were not utilized by any of the isolated strains; putrescine dihydrochloride, cadaverine dihydrochloride, diaminododecane, and n-dodecane were utilized by all of the isolated strains; and all of the isolated strains except DAD 2-3 could utilize dodecylmercaptan. The alkane derivatives that did not serve as ,growth substrates were tested further in oxidation tests using resting cell preparation. Alkane derivatives that are being oxidized by all of the isolated strains are laurylcyanide and dichlorodecane. Dicyanooctane was also oxidized by all of the isolated strains except DAD 30L, chlorodecane was the only oxidized by the three isolated strains. The most remarkable substrate that is being oxidized is dichlorodecane containing CN groups diterminally. Evidence obtained with thin layer chromatography of ,ethyl acetate extracts of culture broth of isolated strains grown in some alkane derivatives shows that these alkane derivatives are degraded.

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A Study on Discriminative Criteria of 6 Kinds of Achyranthis Radix Using HPLC/DAD;Isolation and Identification of 20-hydroxyecdysone from Aclryranthes japonica $N-{AKAI}$ and Comparison of Patterns of Achyranthis Radix from Different Locations by HPLC (HPLC/DAD를 이용한 6종(種) 우슬(牛膝)의 분류기준 연구;우슬(牛膝)(쇠무릎, Achyranthes japonica $N_{AKAI}$)로부터 20-hydroxyecdysone 분리.동정 및 산지별 우슬의 HPLC 패턴 비교)

  • Kim, Jeong-Hi;Kim, Jong-Mun;Kang, Dae-Hoon
    • The Korea Journal of Herbology
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    • v.23 no.1
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    • pp.109-116
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    • 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.

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Development of Quality Control Method for a Novel Herbal Medicine, HPL-1 using UHPLC (UHPLC를 이용한 새로운 한약제제 HPL-1의 품질관리법 개발)

  • Kim, Se-Gun;Lamichhane, Ramakanta;Lee, Kyung-Hee;Jung, Hyun-Ju
    • The Korea Journal of Herbology
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    • v.30 no.3
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    • pp.19-24
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    • 2015
  • Objectives : HPL-1, a novel herbal medicine which is composed of five herbs such as Kalopanacis Cortex, Chaenomelis Fructus, Raphani Semen, Atractylodis Rhizoma and Pulvis Aconiti Tuberis Purificatum, was developed for treatment of osteoarthritis. This study is aimed to develop analytical method for consistent quality control of HPL-1 and validate chromatographic method. Methods : Chromatographic analysis was performed using ultra-high performance liquid chromatography - diode array detector (UHPLC-DAD) equipped with RP-amide column, column oven, and auto sampler. Marker compounds [protocatechuic acid, chlorogenic acid, liriodendrin, 3,5-dicaffeoylquinic acid, ${\beta}$-D-(3-O-sinapoyl)-fructofuranosyl-$\alpha$-D-(6-O-sinapoyl)glucopyranoside and benzoylmesaconine] were separated by step gradient elution of acetonitrile and 0.1% phosphoric acid/water. The method validation was evaluated by quantitative validation parameters of linearity, accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ) according to KFDA guideline.Results : An optimized method for six marker compounds in HPL-1 was established by UHPLC-DAD. The correlation coefficient (R2) with each calibration curve was greater than 0.99. The LOD and LOQ were within the range of 0.008-0.090 and $0.023-0.274{\mu}g/mL$, respectively. The relative standard deviation (RSD) of intra- and inter-day variability were less than 4.0%. The result of recovery test was range from 93.3-106.3% with RSD < 4.0%.Conclusions : These results suggest that the quantitative UHPLC method is precise, accurate, effective for quality evaluation of HPL-1. The method may also contribute to improve quality of crude drug preparations used for treatment of various diseases.