• Title/Summary/Keyword: Flow rate gradient

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Evaluation on Extraction Conditions and HPLC Analysis Method for Bioactive Compounds of Astragali Radix (황기의 추출조건 및 유효성분의 HPLC 분석법 평가)

  • Kim, Geum Soog;Lee, Dae Young;Lee, Seung Eun;Noh, Hyung Jun;Choi, Je Hun;Park, Chun Geun;Choi, Soo Im;Hong, Seung Jae;Kim, Seung Yu
    • Korean Journal of Medicinal Crop Science
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    • v.21 no.6
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    • pp.486-492
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    • 2013
  • This study has been conducted to establish the optimal extraction process and HPLC analysis method for the determination of marker compounds as a part of the materials standardization for the development of health functional food materials from Astragali radix. Five extraction conditions including the shaking extraction at room temperature and the reflux extraction at $85^{\circ}C$ with 30%, 50% and 95% ethanol were evaluated. Reflux extraction with 50% ethanol showed the highest extraction yield as $27.27{\pm}2.27%$, while the extraction under reflux with 95% ethanol showed significantly the lowest yield of $10.55{\pm}0.24%$. The quantitative determination methods of calycosin-7-O-${\beta}$-D-glucoside and calycosin as marker compounds of Astragali radix extracts were optimized by HPLC analysis using a Thermo Hypersil column ($4.6{\times}250mm$, $5{\mu}m$) with the gradient elution of water and acetonitrile as the mobile phase at the flow rate of $0.8mLmin^{-1}$ and a detection wavelength of 230nm. The HPLC/UV method was applied successfully to the quantification of two marker compounds in Astragali radix extracts after validation of the method with the linearity, accuracy and precision. The contents of calycosin-7-O-${\beta}$-D-glucoside and calycosin in 50% ethanol extracts by reflux extraction were significantly higher as $1,700.3{\pm}30.4$ and $443.6{\pm}8.4{\mu}g-1$, respectively, comparing with those in other extracts. The results indicate that the reflux extraction with 50% ethanol at $85^{\circ}C$ is optimal for the extraction of Astragali radix, and the established HPLC method are very useful for the evaluation of marker compounds in Astragali radix extracts to develop the health functional material from Astragali radix.

Validation of Analytical Method of Marker Compounds in Extract of Pear Pomace as a Functional Health Ingredient (건강기능식품 원료로서 나주 배박 추출물의 지표성분 분석법 벨리데이션)

  • Cho, Eun-Jung;Bang, Mi-Ae;Cho, Seung-Sik
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.11
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    • pp.1682-1686
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    • 2015
  • This study was conducted to establish an HPLC analysis method for determination of marker compounds as part of materials standardization for development of health functional food materials from pear pomace. The quantitative determination method of caffeic acid and chlorogenic acid as marker compounds of pear pomace extract (PPE) was optimized by HPLC analysis using a C18 column ($5{\times}250mm$, $5{\mu}m$) with a 0.2% elution gradient of acetic acid and methanol as the mobile phase at a flow rate of 0.8 mL/min and detection wavelength of 330 nm. The HPLC/UV method was applied successfully to the quantification of marker compounds in PPE after validation of the method with linearity, accuracy, and precision. The method showed high linearity of the calibration curve with a coefficient of correlation ($R^2$) of 0.9999, and limit of detection and limit of quantification were $1.14{\mu}g/mL$ (caffeic acid) and $1.61{\mu}g/mL$ (chlorogenic acid) as well as $4.9{\mu}g/mL$ (caffeic acid) and $4.9{\mu}g/mL$ (chlorogenic acid), respectively. Relative standard deviation values from intra- and inter-day precision were less than 3.1% (caffeic acid) and 4.0% (chlorogenic acid), respectively. Recovery rates of caffeic acid and chlorogenic acid at 12.5, 25, and $50{\mu}g/mL$ were 93.66~106.32% and 97.33~105.68%, respectively. An optimized method for extraction of caffeic acid and chlorogenic acid in PPE was established through diverse extraction conditions, and the validation indicated that the method is very useful for evaluation of marker compounds in PPE to develop a health functional food material.

Analysis of Oxygen Combustion Characteristics of a Low Grade Coal Using IEA-CFBC Model (IEA-CFBC 모델을 이용한 저급탄의 순산소 연소 특성 분석)

  • Gwak, You Ra;Kim, Ye Bin;Keel, Sang In;Yun, Jin Han;Lee, See Hoon
    • Korean Chemical Engineering Research
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    • v.56 no.5
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    • pp.631-640
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    • 2018
  • The application of an oxy-combustion circulating fluidized bed combustor (Oxy-CFBC) for low grade coals has recently developed in the world to meet the continuous increase of energy demand and to achieve the reduction of greenhouse gases. Since demo plants for Oxy-CFBC have been developed, the combustion properties of Oxy-CFBC in various operation conditions, such as gas flow rates, combustion temperature, fuel, and so on, should be investigated to develop design criteria for a commercial Oxy-CFBC. In this study, a computational simulation tool for Oxy-CFBC was developed on the basis of the IEA-CFBC (International Energy Agency Circulating Fluidized Bed Combustor) model. Simulation was performed under various conditions such as reaction temperature ($800^{\circ}C{\sim}900^{\circ}C$), oxygen contents (21%~41%), coal feeding rate, Ca/S mole ratio (1.5~4.0), and so on. Simulation results show that the combustion furnace temperature is higher in oxy 1 than air fired. However, the temperature gradient tended to decrease with increasing oxy mixing percent. In case of $SO_x$, the higher the Ca/S mole ratio and oxy mixing percent, the higher the desulfurization efficiency.

Validation of Method Determining Marmesin in Broussonetia kazinoki Extract (닥나무 추출물의 Marmesin 성분 분석법 검증)

  • Kwon, Jin Gwan;Seo, Changon;Hong, Seong Su;Seo, Dong-Wan;Oh, Joa Sub;Kim, Jin Kyu
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.11
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    • pp.1604-1609
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    • 2016
  • An HPLC analysis method was developed for standard determination of marmesin as a functional health material in Broussonetia kazinoki extract. HPLC was performed on a $C_{18}$ Kromasil column ($4.6{\times}250mm$, $5{\mu}m$) with a gradient elution of 0.1% (v/v) trifluoroacetic acid and acetonitrile at a flow rate of 1.0 mL/min at $30^{\circ}C$. The analyte was detected at 330 nm. The HPLC method was validated in accordance with International Conference on Harmonization guidelines for analytical procedures with respect to specificity, precision, accuracy, and linearity. The limit of detection and quantitation were 6.2 and $18.6{\mu}g/mL$, respectively. Calibration curves showed good linearity ($r^2$>0.9999), and the precision of analysis was satisfactory (less than 0.3%). Recoveries of quantified compound ranged from 100.35 to 101.18%. This result indicates that the established HPLC method is very useful for the determination of marker compounds in B. kazinoki extracts.

Validation of the LC-MS/MS Method for Ginsenoside Rb1 Analysis in Human Plasma (LC-MS/MS를 이용한 인체 혈장에서 Ginsenoside Rb1의 분석법 검증)

  • Han, Song-Hee;Kim, Yunjeong;Jeon, Ji-Young;Hwang, Minho;Im, Yong-Jin;Lee, Sun Young;Chae, Soo-Wan;Kim, Min-Gul
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.41 no.12
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    • pp.1753-1757
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    • 2012
  • A new liquid chromatographic tandem mass spectrometric (LC-MS/MS) assay for the quantification of ginsenoside Rb1 in human plasma was developed and validated. The separation was performed on a Agilent C18 column ($4.6mm{\times}150mm$, particle size 5 ${\mu}m$) with a gradient elution of 0.1% formic acid in water and 0.1% formic acid in methanol and a flow rate of 0.9 mL/min. The analyte was determined using electrospray positive ionization mass spectrometry in the multiple reaction monitoring (MRM) mode (m/z 1131.714${\rightarrow}$365.303). Human plasma samples were extracted with acetone : water (50:50) by the liquid-liquid extraction method. The method was linear over the dynamic range of 10~500 ng/mL with a correlation coefficient of r=0.9995. The intra-and inter-day precision over the concentration range of ginsenoside Rb1 was lower than 5.8% (correlation of variance, CV), and the accuracy was between 96.0~104.6%. This LC-MS/MS assay of ginsenoside Rb1 in human plasma is applicable for quantification in a pharmacokinetic study.

Characteristics of Waterlevel Fluctuation in Riverside Alluvium of Daesan-myeon, Changwon City (창원시 대산면 강변충적층의 지하수위 변동 특성)

  • Cheong, Jae-Yeol;Hamm, Se-Yeong;Kim, Hyoun-Su;Son, Keon-Tae;Cha, Yong-Hoon;Jang, Seong;Baek, Keon-Ha
    • The Journal of Engineering Geology
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    • v.13 no.4
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    • pp.457-474
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    • 2003
  • This study aims to elucidate characteristics of groundwater level fluctuation at riverbank filtration sites in Daesan-myeon, Changwon City. Groundwater level fluctuation, river water level change and stream-aquifer interaction are very important to estimate optimal discharge rate of the pumping well. Water level contours from February 2003 to October 2003 show normal decreasing trend toward the Nakdong river with the hydraulic gradient of 0.008. However, flow reversion occurs when groundwater is discharged at the pumping wells or rise of the Nakdong river by rainfall. The fluctuation of the Nakdong river ranges 0 - 10 m msl. Autocorrelation analysis was conducted to the groundwater levels measured on the six monitoring wells (DS1, DS2, DS3, DS4, DS6 and DS7). The analyzed waterlevel data can be grouped into three: group 1 (DS1 and DS3) represents strong linearity and long memory effect, group 2 (DS1 and DS6) intermediate linearity and memory, and group 3 (DS4 and DS7) weak linearity and memory. Waterlevels of group 1 wells are relatively closely related to the change of river-water level. Those of group 2 wells are largely affected by the pumping and the river-water level, and those of group 3 wells are strongly linked to pumping.

Validation of an analytical method of dieckol for standardization of Ecklonia cava extract as a functional ingredient (감태추출물의 기능성원료 표준화를 위한 지표성분 dieckol의 분석법 검증)

  • Xu, Yan;Kim, Eun Suh;Lee, Ji-Soo;Kim, Gun-Hee;Lee, Hyeon Gyu
    • Korean Journal of Food Science and Technology
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    • v.51 no.5
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    • pp.420-424
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    • 2019
  • An HPLC analysis method was developed and standardized for the detection of dieckol as a functional food ingredient in Ecklonia cava extracts. HPLC was performed using a Capcell Pak C18 column ($250{\times}4.6mm$, $5{\mu}m$) with a gradient elution of water and acetonitrile, both containing 0.1% (v/v) trifluoroacetic acid, at a flow rate of 1.0 mL/min at $25^{\circ}C$. The eluate was detected at 230 nm. For validation, the specificity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ) of dieckol were measured. The calibration curve for the detection of dieckol had high linearity ($R^2=0.9994$), with LOD and LOQ values of 0.38 and $1.16{\mu}g/mL$, respectively. Recovery of the quantified compound ranged from 99.61 to 100.71%. The relative standard deviation values of the intra-day and inter-day precisions were less than 1.7 and 1.25%, respectively. These results indicate that the reported HPLC method is simple, reliable, and reproducible for the detection of dieckol in Ecklonia cava extracts.

Analytical Method Development of (-)-Epicatechin gallate in Penthorum chinense Pursh Extract using HPLC (HPLC를 이용한 낙지다리 추출물의 (-)-­Epicatechin gallate 분석법 개발)

  • Kwon, Jin Gwan;Jung, Yeon Woo;Seo, Changon;Hong, Seong Su;Choi, Chun Whan;Lee, Ji Eun;Shin, Hyun Tak;Jung, Su Young;Kim, Jin Kyu
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.45 no.1
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    • pp.87-93
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    • 2019
  • This study attempted to eatablish a High Performance Liquid Chromatography (HPLC) analysis method for the determination of (-)-epicatechin gallate as a part of the quality control for the development of functional cosmetic materials from Penthorum chinense Pursh. HPLC was performed on a Unison $US-C_{18}$ column ($4.6{\times}250mm$, $5{\mu}m$) with a gradient elution of 0.05% (v/v) trifluoroacetic acid (TFA) and methyl alcohol at a flow rate of 1.0 mL/min at $30^{\circ}C$. The analyte was detected at 280 nm. The HPLC method was performed in accordance with the International Conference on Harmonization (ICH) guideline (version 4, 2005) of analytical procedures with respect to specificity, precision, accuracy, and linearity. The limits of detection and quantitation were 0.11 and 0.33 mg/mL, respectively. Calibration curves showed good linearity ($r^2$ > 0.9999), and the precision of analysis was satisfied (less than 0.6%). Recoveries of quantified compounds ranged from 99.51 to 101.92%. This result indicates that the established HPLC method is very useful for the determination of marker compound in P. chinense Pursh extracts.

Development and validation of an LC-MS/MS method for the simultaneous analysis of 26 anti-diabetic drugs in adulterated dietary supplements and its application to a forensic sample

  • Kim, Nam Sook;Yoo, Geum Joo;Kim, Kyu Yeon;Lee, Ji Hyun;Park, Sung-Kwan;Baek, Sun Young;Kang, Hoil
    • Analytical Science and Technology
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    • v.32 no.2
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    • pp.35-47
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    • 2019
  • In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak(R) C18 MG-II ($2.0mm{\times}100mm$, $3{\mu}m$), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with $R^2$ > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.

Characteristics of Channelbed and Woody Debris on Mountainous Stream (산지급류소하천(山地急流小河川)에 있어서 하상미지형(河床微地形)과 유목(流木) 특성(特性))

  • Chun, Kun-Woo;Kim, Min-Sik;Park, Wan-Geun;Ezaki, Tsugio
    • Journal of Korean Society of Forest Science
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    • v.86 no.1
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    • pp.69-79
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    • 1997
  • The purpose of this study is to acquire essential data to reduce the amount of woody debris resulted from the debris flow. This research examined topographic characteristics of the channelbed affecting generation, movement and storage of woody debris and woody characteristics related to number, sizes, shapes, decay, storage direction to mountainous stream. 1. The number of woody debris had a tendency to increase in proportion to stream width, but it was hardly affected by longitudinal gradient of stream. Especially, the greater amount of woody debris was stored at wide section of the stream with compound channel, and it was found in deposits of channelbed rather than in the present channel. 2. Total woody debris over 10cm in diameter and over 2m in length was 402 units and storage number was 35.3 units per 100m of stream. Average diameter of breast height and length were 14cm and 4m, respectively. The woody debris appeared shorter in length and greater in diameter at down-stream than up-stream. 3. Since woody debris met sediments and bed-materials of great roughness in moving, the greater amount of woody debris without root was found in up-stream and down-stream, but deformed woody debris was discovered in upper stream. Decay of woody debris was more severe in down-stream and woody debris on rotting process was found down-stream. 4. Storage direction of woody debris was mainly parallel to center line of stream, and rate of parallel and perpendicularity was 276 and 126 units, respectively. But, as woody debris storing to the perpendicular direction was unstable, the traveling debris could easily be stored. Therefore, some counterplan was required to prevent the traveling woody debris. 5. Tree species of woody debris was mainly larch, which occupied about two third of total woody debris(256 units). The woody debris of larch is easy to move due to hitting of channelbed materials or lower channelbed fluctuation because the lower part of larch is weaker than its upper part. Therefore, the section of the tree species planting in the riparian vegetation needs much more carefulness.

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