• 제목/요약/키워드: Gradient array

검색결과 136건 처리시간 0.018초

Quality Evaluation of Modified Bo-Yang-Hwan-O-Tang by Capillary Electrophoresis and High-performance Liquid Chromatography

  • Chen, Jianbo;Wu, Enqi;Zhu, Hongmei;Lee, Kwan-Jun;Chu, Van Men;Cho, Cheong-Weon;Kim, Young-Ho;Park, Yong-Ki;Lee, Won-Jae;Kang, Jong-Seong
    • Bulletin of the Korean Chemical Society
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    • 제32권8호
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    • pp.2666-2670
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    • 2011
  • High-performance liquid chromatography (HPLC) and capillary electrophoresis (CE) were used to identify five active components in the modified herbal decoction Bo-Yang-Hwan-O-Tang (mBHT), i.e., amygdalin, decursin, paeoniflorin, salvianolic acid B, and calycosin-7-O-${\beta}$-D-glycoside. These components were identified by comparing their retention times and mass spectra with those of reference compounds. The conditions of both analytical methods were optimized and validated. Sufficient separation of target analytes was achieved using a buffer consisting of 40 mM sodium borate and 60 mM sodium dodecylsulfate (SDS) containing 10% methanol (pH 9.5) at 250 nm for CE analysis and gradient elution with a water-methanol mobile phase and ultraviolet (UV) photodiode array detector (DAD) at 250 nm for HPLC analysis. The mBHT components were determined within 65 min by HPLC and 16 min by CE. All calibration curves showed high linearity (R > 0.999) within the ranges tested. Intra-day and inter-day precision were less than 1.6% and 1.8% for HPLC and 2.5% and 4.8% for CE, respectively. The accuracy of the methods ranged from 98.8% to 102.3% for HPLC and from 95.9% to 108.2% for CE.

HPLC를 이용한 발효 감초의 지표 성분 분석 (Quantitative Analysis of Glycyrrhizic Acid in Fermented Glycyrrhizae Radix by HPLC)

  • 엄영란;심기석;이재훈;박화용;마진열
    • 한국한의학연구원논문집
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    • 제15권1호
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    • pp.85-89
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    • 2009
  • The aim of this study was to study the quantitative analysis of glycyrrhizic acid in Glycyrrhizae Radix extract fermented with Paecilomyces japonica, Ganoderma lucidum, honey or Nuruk. The amounts of dry on loss were measured and the quantitative analysis of glycyrrhizic acid was performed by high performance liquid chromatographic (HPLC). HPLC method was performed on C18 column ($250\;mm\;{\times}\;4.6\;mm$, $5\;{\mu}m$, RS tech) using gradient solvent mixtures of water-acetonitrile with photodiode array detector (254 nm). The flow rate was $1.0\;m{\ell}/min$. Retention time of glycyrrhizic acid was about 23.96 min and linearity of calibration was $R^2$=0.9998. Contents of glycyrrhizic acid in Glycyrrhizae Radix extract (control) was $5.048\;{\pm}\;0.14$; Contents of glycyrrhizic acid in Glycyrrhizae Radix extract fermented with Paecilomyces japonica (SDT) was $1.975\;{\pm}\;0.07$; Contents of glycyrrhizic acid in Glycyrrhizae Radix extract fermented with Ganoderma lucidum (SYT) was $2.676 \;{\pm}\;0.07$; Contents of glycyrrhizic acid in Glycyrrhizae Radix extract fermented with honey (SST) was $5.191\;{\pm}\;0.06$; Contents of glycyrrhizic acid in Glycyrrhizae Radix extract fermented with Nuruk (SNT) was $5.305\;{\pm}\;0.34$, respectively. Contents of glycyrrhizic acid in SDT and SYT were decreased but that in SST and SNT was increased when compared to control.

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마이크로채널 내의 온도 분포 측정을 위한 미소 측정 구조물의 제작 (Fabrication of a novel micromachined measurement device for temperature distribution measurement in the microchannel)

  • 박호준;임근배;손상영;송인섭;박정호
    • 대한전기학회:학술대회논문집
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    • 대한전기학회 2001년도 하계학술대회 논문집 C
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    • pp.1921-1923
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    • 2001
  • In this work, an array of resistance temperature detector(RTD) was fabricated inside the microchannel in order to investigate in-situ flow characteristics. A rectangular straight microchannel, integrated with RTD's for temperature sensing and a heat source for generating the temperature gradient along the channel. were fabricated with the dimension of $200{\mu}m(W){\times}{\mu}m(D){\times}$48mm(L), while RTD measured precise temperatures at the inside-channel wall. 4" $525{\pm}25{\mu}m$ thick P-type <100> Si wafer was used as a substrate. For the fabrication of RTDs. 5300$\AA$ thick Pt/Ti layer was sputtered on a Pyrex glass wafer. Finally, glass wafer was bonded with Si wafer by anodic bonding, therefore RTD was located inside the microchannel. The temperature distribution inside the fabricated microchannel was obtained from 4 point probe measurements and Dl water is used as a working fluid. Temperature distribution inside the microchannel was measured as a function of mass flow rate and heat flux. As a result, precise temperatures inside the microchannel could be obtained. In conclusion, this novel temperature distribution measurement system will be very useful to the accurate analysis of the flow characteristics in the microchannel.

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HPLC-PDA을 이용한 이진탕 중 6종 성분의 동시분석 (Simultaneous Analysis of Six Compounds in Yijin-tang by HPLC-PDA)

  • 김성실;김정훈;신현규;서창섭
    • 대한한의학방제학회지
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    • 제21권1호
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    • pp.71-79
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    • 2013
  • Objectives : Yijin-tang has been used in the treatment of gastrointestinal diseases such as irritable bowel syndrome, gastritis, and gastric ulcer. In this study, a high-performance liquid chromatography (HPLC) method was established for simultaneous analysis of six compounds, liquiritin, glycyrrhizin, hesperidin, 6-gingerol, homogentisic acid, and 3,4-dihydroxybenzaldehyde in Yijin-tang, a traditional Korean herbal medicinal preparation. Methods : A Gemini C18 column was used for the separation of six constituents at $40^{\circ}C$. The mobile phase using gradient elution consist of two solvent systems, 1.0% acetic acid in water (A) and 1.0% acetic acid in acetonitrile (B). The flow-rate was 1.0 mL/min and injection volume was $10{\mu}g$. The detector was a photodiode array (PDA) detector set at 254 nm and 280 nm. Results : The calibration curves of six compounds showed good linearity in various concentration ranges ($R^2{\geq}0.9997$). The limits of detection (LOD) and limits of quantification (LOQ) were 0.028-$0.192{\mu}g/mL$ and 0.093-$0.540{\mu}g/mL$, respectively. The RSD (%) of the intra and inter day validations were 0.03-0.84% and 0.05 -1.00%, respectively. Recovery was 96.14-01.90% and RSD (%) was less than 1.5%. Conclusions : The established simultaneous analysis methods will help management to improve the quality of Yijin-tang.

Evaluation of the Immune-Stimulating Activity of Samul-tang, a Traditional Korean Herbal Medicine, Standardized by HPLC-PDA

  • Seo, Chang-Seob;Ha, Hye-Kyung;Jung, Da-Young;Lee, Ho-Young;Shin, Hyeun-Kyoo
    • 대한한의학회지
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    • 제32권3호
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    • pp.25-34
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    • 2011
  • Objectives: We performed simultaneous determination of five constituents by HPLC in Samul-tang (SMT). Additionally, we investigated the immune-stimulatory potential of SMT on specific cellular and humoral immune responses in ovalbumin (OVA)-immunized mice. Methods: Reverse-phase chromatography using a Gemini C18 column operating at $40^{\circ}C$, and photodiode array (PDA) detection at 190-400 nm, were used for quantification of the five components of SMT. Mobile phase using a gradient flow consisted of two solvent systems. Solvent A was 1.0% (v/v) aqueous acetic acid and solvent B was acetonitrile with 1.0% (v/v) acetic acid. C57BL/6 mice were immunized intraperitoneally with OVA/alum ($100{\mu}g/200{\mu}g$) on days 1, 8, and 15. The extract of SMT (1000 mg/kg) was given to mice orally for 21 days (from day 1 to day 21). At day 22, OVA-, lipopolysaccharide (LPS)- and concanavalin A (Con A)-stimulated splenocyte proliferation and OVA-specific and total antibodies were measured in plasma. Results: Calibration curves were acquired with $r^2$>0.9999, and the relative standard deviation (RSD, %) for intra- and inter-day precision were both less than 3.5%. The recovery was in the range of 95.69-115.12%, with an RSD less than 6.0%. The contents of five components in SMT were 1.08-15.30 mg/g. SMT significantly enhanced Con A-induced splenocyte proliferation in OVA-immunized mice (p<0.01). Also, SMT significantly enhanced OVAspecific IgG, IgG1 and total IgM levels in plasma compared with the OVA-immunized group. Conclusions: The established method will be applied for the quantification of major components and immunestimulating activity in OVA-immunized mouse model of SMT.

HPLC-PDA를 이용한 오약순기산 중 6종 성분의 동시분석 (Simultaneous Analysis of Six Constituents in Oyaksungi-san using HPLC-PDA)

  • 서창섭;김정훈;신현규
    • 대한한의학방제학회지
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    • 제20권2호
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    • pp.37-46
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    • 2012
  • Objectives : Oyaksungi-san(Wuyaoshunqisan) has been used for treatment of stroke and rheumatoid arthritis in Korea. In this study, a simple and accurate high-performance liquid chromatography(HPLC) method was established for simultaneous determination of six main components, liquiritin, ferulic acid, naringin, hesperidin, neohesperidin, and glycyrrhizin in Oyaksungi-san, a traditional Korean herbal prescription. Methods : The analytical column for separation of six constituents was used a Gemini $C_{18}$ column maintained at $40^{\circ}C$. The mobile phase consisted of two solvent systems, 1.0% (v/v) acetic acid in $H_2O$ (A) and 1.0% (v/v) acetic acid in acetonitrile (B) by gradient flow. The flow rate was 1.0 mL/min and the detector was a photodiode array (PDA) set at 254 nm for glycyrrhizin, 280 nm for liquiritin, naringin, hesperidin, and neohesperidin, and 320 nm for ferulic acid. Results : Calibration curves were acquired with $r^2$ values ${\geq}0.9998$. The results of recovery test were 91.58%-105.90% with a relative standard deviations (RSDs, %) value less than 2.0%. The values of RSD for intra- and inter-day precision were 0.03%-1.72% and 0.03%-1.63%, respectively. The contents of the six compounds in Oyaksungi-san were 0.33-9.30 mg/g. Conclusions : The newly established HPLC method will be helpful to improve quality control of Oyaksungi-san.

선형 위상 특성을 갖는 적응 마이크로폰 어레이 (An Adaptive Microphone Array with Linear Phase Response)

  • 강홍구;윤대희;차일환
    • 한국음향학회지
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    • 제11권3호
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    • pp.53-60
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    • 1992
  • 원거리 회의나 대강당 등의 회의에서 주변의 간섭 잡음을 제거하고 정해진 발언자의 음성 신호를 얻기 위하여 적응 빔 형성 기법을 이용한 방법이 연구되어 왔다. 음성 신호에 이용되는 적응 빔 기법은 레이더, 소나, 지진파 신호의 경우와는 달리 어느 정도 왜곡이 있더라도 출력 신호가 인간의 청각 특성에 적합해야 한다. Sondhi는 인간의 귀가 음성 신호의 위상에는 민감하지 않다는 성질을 이용하여 음성의 크기에 약한 제한 조건을 갖는 cost 함수를 정의하고, 이를 gradient 탐색 알고리즘을 사용하여 최적화된 필터계수를 구했다. 본 논문에서는 Sondhi가 제안한 빔 형성기의 위상 왜곡에 따른 음절 저하를 극복하기 위해 원하는 신호 방향에 대해서 선형 위상 응답 특성을 갖는 빔 형성기를 제안하였으며, 실제로 시스템을 구현할 경우 효과적으로 이용할 수 있는 샘플 처리 알고리듬을 제안하였다. 제안된 알고리듬의 성능 평가를 위하여 컴퓨터 시뮬레이션을 수행하였다.

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

  • 김세건;라마칸타라미차네;이경희;정현주
    • 대한본초학회지
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    • 제30권3호
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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.

Simultaneous Determination of Six Components in the Traditional Herbal Medicine 'Oryeongsan' by HPLC-DAD and LC-MS/MS

  • Lee, Jiwoo;Weon, Jin Bae;Lee, Bohyoung;Yun, Bo-Ra;Eom, Min Rye;Ma, Choong Je
    • Natural Product Sciences
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    • 제19권1호
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    • pp.20-27
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    • 2013
  • A simple high performance liquid chromatography - diode array detector (HPLC-DAD) method has been developed and validated for simultaneous determination of the six components (cinnamic acid, cinnamaldehyde, eugenol, atractylenolide I, atractylenolide III, and ergosterol) in Oryeongsan. In addition, identification of six marker compounds was conducted by a LC-MS/MS analysis. The six compounds in Oryeongsan were separated on Shishedo $C_{18}$ column (5 ${\mu}m$, $4.6{\times}250$ mm) at a column temperature of $30^{\circ}C$. The mobile phase was a mixture of 0.1% trifluoroacetic acid (TFA) water and acetonitrile employing gradient elution at a flow rate of 1.0 mL/min. The detection wavelength was set at 205, 250, 280, and 330 nm. The developed method had good linearity ($R^2$ > 0.9997) and the limit of detection (LOD) and limit of quantification (LOQ) were observed within the ranges 0.01~0.15 and 0.05~0.45 ${\mu}g/mL$, respectively. The relative standard deviation (RSD) values of intra- and inter-day testing were indicated that less than 3% and 90.31~103.31% of accuracy. The results of recovery test were 90.56~106.72% and RSD range was measured from 0.84 to 2.95%. In conclusion, this HPLC-DAD method has been successfully applied to the simultaneous determination of six compounds in Oryeongsan samples.

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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    • 제26권1호
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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.