• Title/Summary/Keyword: Precision Rate

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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.

Simultaneous Determination of Pesticides in Water Using a GC/MS Coupled with Micro Extraction by Packed Sorbent (MEPS-GC/MS를 이용한 농약류 동시 수질분석)

  • Lee, Ki-chang;Lee, Wontae
    • Journal of Korean Society of Environmental Engineers
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    • v.37 no.5
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    • pp.262-268
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    • 2015
  • This study established an analytical method to simultaneously determine six organophosphorous pesticides [methyldemetone-S, diazinon, fenitrothion, parathion, phentoate, and O-ethyl O-(4-nitrophenyl) phenylphosphonothioate (EPN)] and carbaryl in water using a gas chromatography/mass spectrometry (GC/MS) system coupled with on-line micro extraction by packed sorbent (MEPS) and programmed temperature vaporizer (PTV) injector. Polystyrene divinylbenzene (PDVB) was used as a sorbent of MEPS. The effects of elution solvents, pH, elution volume and draw-eject cycles of samples on sample pretreatment process were investigated. Also, quality assurance and quality control (QA/QC) and the recovery of the pesticides in environmental samples were evaluated. The elution was performed using $30{\mu}L$ of a mixed solvent (acetone : dichloromethane = 80 : 20 (v/v)). Sample pretreatment processes were optimized with seven cycles of draw-eject of sample (1 mL) spiking an internal standard and sulfuric acid. At lower pH, the analytical sensitivity of diazinon decreased, but that of carbaryl increased. The method detection limit and the limit of quantification for this method were 0.02~0.18 and $0.08{\sim}0.59{\mu}g/L$, respectively. The method precision and accuracy were 1.5~11.5% and 83.3~129.8%, respectively, at concentrations of $0.5{\sim}5.0{\mu}g/L$. The recovery rates for all the pesticides except carbaryl in various environmental samples ranged 75.7~129.3%. The recovery rate of carbaryl in effluent sample was over 200% whereas carbaryl in drinking water, groundwater, and river water were in the acceptable range.

The Development of Growth and Yield Models for the Natural Broadleaved-Korean Pine Forests in Northeast China (중국(中國) 동북부(東北部) 지방(地方) 활엽수(闊葉樹)-잣나무 천연림(天然林)의 생장(生長) 모델과 수확(收穫) 모델 개발(開發))

  • Li, Fengri;Choi, Jung-Kee;Kim, Ji-Hong
    • Journal of Korean Society of Forest Science
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    • v.90 no.5
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    • pp.650-662
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    • 2001
  • The growth and yield models for five different kinds of natural forest types were systemically developed in the natural Broadleaved-Korean pine Forests in Northeast China. The data were collected from 359 temporary plots and 58 permanent plots with area ranged from 0.06 ha to 1.0 ha, ranging in stand age from 43 to 364 years. The Site Class Index (SCI) was introduced to evaluate site quality and the Crown Competition Factor (CCF) was selected as a measure of stand density for the mixed natural forest. The Chapman-Richards function was adopted to develop SCI equation and height-diameter curve. The Schumacher growth function was selected as base model to develop the DBH, basal area, and stand volume growth models by using re-parameterized method. In modeling mean DBH and basal area growth, it was found that the asymptotic parameter A of Schumacher function was exponentially related to site quality (SCI) and stand density (CCF). The rate parameter k was related to stand density and it was independent of SCI. Several validation measures for predicted stand variables were evaluated in the growth and yield models using independent data sets. The results indicated that relative mean errors (RME) in predicted stand attributes were less than ${\pm}5%$ and the estimated precision values of the stand variables were all greater than 95%.

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Design of a Low Power Digital Filter Using Variable Canonic Signed Digit Coefficients (가변 CSD 계수를 이용한 저전력 디지털 필터의 설계)

  • Kim, Yeong-U;Yu, Jae-Taek;Kim, Su-Won
    • Journal of the Institute of Electronics Engineers of Korea SD
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    • v.38 no.7
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    • pp.455-463
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    • 2001
  • In this Paper, an approximate processing method is proposed and tested. The proposed method uses variable CSD (VCSD) coefficients which approximate filter stopband attenuation by controlling the precision of the CSD coefficient sets. A decimation filter for Audio Codec '97 specifications has been designed having processor architecture that consists of program/data memory, arithmetic unit, energy/level decision, and sinc filter blocks, and fabricated with 0.6${\mu}{\textrm}{m}$ CMOS sea-of-gate technology. For the combined two halfband FIR filters in decimation filter, the number of addition operations were reduced to 63.5%, 35.7%, and 13.9%, compared to worst-case which is not an adaptive one. Experimental results show that the total power reduction rate of the filter is varying from 3.8 % to 9.0 % with respect to worst-case. The proposed approximate processing method using variable CSD coefficients is readily applicable to various kinds of filters and suitable, especially, for the speech and audio applications, like oversampling ADCs and DACs, filter banks, voice/audio codecs, etc.

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Analytical Method Validation of Quercetin in Changnyeong Onion Extract as a Functional Ingredient for Functional Health Food (건강기능식품 기능성원료로서 창녕양파추출액의 지표성분 Quercetin 분석법)

  • Jeon, Seon-Young;Jeong, Eun-Jeong;Baek, Jeong-Hwa;Cha, Yong-Jun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.40 no.4
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    • pp.565-569
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    • 2011
  • Validation of quercetin as a marker compound in the standardization of Changnyeong onion extract developed for functional health food was attempted by analytical method. The specificity was satisfied with retention time and photo diode array (PDA) spectrum by analysis of quercetin using HPLC and comparison with standard compound. It showed a high linearity in the calibration curve as coefficient of correlation ($R^2$) of 0.9986, and the limit of detection (LOD) and limit of quantitation (LOQ) were 0.2 mg/L and 0.5 mg/L, respectively. Recovery rate test with quercetin concentration of 0.05, 0.075 and 0.1 mg/mL was revealed in the high range of 82.36~95.26%, 82.70~98.24% and 87.91~95.11%, respectively. The intra-day and inter-day precision in quercetin for Changnyeong onion extracts was 0.10~3.28% and 0.96~5.79%, respectively. Therefore, application of quercetin was validated in analytical method as a marker compound in Changnyeong onion extracts.

Quantification of Entacapone in Human Plasma by HPLC Coupled to ESI-MS/MS Detection: Application to Bioequavalence Study (체외에서 ESI-MS/MS 탐지에 연결된 HPLC에 의한 Entacapon의 수량화: 생물학적 동등성 연구에 적용)

  • Balasekhara Reddy., Ch.;Baburao., Ch.;Chandrasekhar., K.B.;Kanchanamala., K.;RihanaParveen., S.K.;Ravikumar., Konda
    • Journal of the Korean Chemical Society
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    • v.54 no.5
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    • pp.523-532
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    • 2010
  • The proposed method is simple, sensitive and specific Liquid chromatography-tandem mass spectrometry (LCESI-MS/MS) method for the quantification of Entacapone (EA) in human plasma using Entacapone-d10 (EAD10) as an internal standard (IS). Chromatographic separation was performed on Zorbax SB-C18, $2.1{\times}50\;mm$, $5\;{\mu}m$ column, mobile phase composed of 10 mM Ammonium formate (pH 3.0): Acetonitrile (60:40 v/v), with a flow-rate of 0.7 mL/min, followed by Liquid-liquid extraction. EA and EAD10 were detected with proton adducts at m/z $306.1{\rightarrow}233.1$ and $316.3{\rightarrow}233.0$ in multiple reaction monitoring (MRM) positive mode respectively. The method was validated over a linear concentration range of 1.00 - 2000.00 ng/mL with correlation coefficient ($r^2$) $\geq$ 0.9993. Intra and inter-day Precision within 3.60 to 7.30 and 4.20 to 5.50% and Accuracy within 97.30 to 104.20 and 98.30 to 105.80% proved for EA. This method is successfully applied in the bioequivalence study of healthy Indian human volunteers.

A Retrospective Review of Tracheobronchial Foreign Bodies (기도 이물의 임상적 고찰)

  • Son, Chang-Young;Wee, Jeong-Ook;Kim, Soo-Ock;Oh, In-Jae;Park, Chang-Min;Kim, Kyu-Sik;Kim, Yu-Il;Lim, Sung-Chul;Lim, Sang-Chul;Kim, Young-Chul;Park, Kyung-Ok
    • Tuberculosis and Respiratory Diseases
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    • v.58 no.6
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    • pp.600-606
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    • 2005
  • Background : The development of bronchoscopic equipment along with the precision of radiographic techniques had reduced the mortality rate of patients with tracheobronchial foreign bodies but has been no change in the incidence of tracheobronchial foreign bodies since their introduction. The aim of this study was to assess the clinical characteristics of a tracheobronchial foreign body aspiration and to evaluate the efficacy of the treatment modality in children and adults. Methods : This is a retrospective review of 64 patients who underwent bronchoscopic procedures for the treatment of aspirated foreign bodies from December 1994 through March 2004 at the Chonnam national university hospital. Results : There were 47 males and 17 females, aged from 1 month to 78 years. Most of the patients had no underlying illness except for one patient with a cerebrovascular accident that contributed to the foreign body aspiration. The most common symptom was cough, which was noted in 54 patients (84.3%). The other presenting symptoms were dyspnea (48.8%), fever (20.3%), sputum (14%), vomiting (7.8%), and chest pain (4.6%). Those whose tracheobronchial foreign bodies were diagnosed more than 2 days after the aspiration (21 patients) were more likely to have pneumonia than those whose foreign bodies were diagnosed within 2 days (p = 0.009). Foreign bodies were visualized in the plain chest radiographs in 12 cases (18.8%), while others showed air trapping (21, 32.8%), pneumonia (15, 23.4%), atelectasis (7, 10.9%), and normal findings (9, 14.1%). The foreign bodies were more frequently found in the right bronchial tree (36) compared with the left bronchial tree (22, p = 0.04). In order to remove the foreign bodies, twenty (31.2%) cases were removed using flexible bronchoscopy, while 42 (65.6%) and 2 (3.2%) cases required rigid bronchoscopy and surgery, respectively. Conclusions : Tracheobronchial Foreign body aspiration had a bimodal age distribution in the infancy and old age around 60 years. They were found more frequently in the right bronchial tree. In addition, patients whose foreign bodies were diagnosed more than 2 days after the aspiration were more likely have a infection. Rigid bronchoscopy is the procedure of choice for uncooperative children and for those with foreign bodies lodged deeply in the small bronchial tree.

HPLC analytical method validation of Aralia elata extract as a functional ingredients (두릅 추출물의 기능성 원료 표준화를 위한 HPLC 분석법 검증)

  • Ahn, Eun-Mi;Choi, Song-Am;Choi, Ji-Young
    • Food Science and Preservation
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    • v.24 no.6
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    • pp.795-801
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    • 2017
  • Aralia elata Seemann (AE) has long been used as a folk medicine for the treatment of various diseases including diabetes mellitus, anti-arthritic, and anti-gastric ulcer agent in Korea, Japan, and China. This study was performed to establish a simple and reliable HPLC/UV analytical method for determination of most active anti-hypertensive compound, a 3-O-${\alpha}$-L-rhamnopyranosyl($1{\rightarrow}$2)-${\alpha}$-L-arabinopyranosyl hederagenin 28-O-${\beta}$-D-xylopyranosyl($1{\rightarrow}6$)-${\beta}$-D-glucopyranosylester (HE) for the standardization of the shoot extract of AE as a health functional food ingredient. The quantitative analytical method of HE was optimized by HPLC analysis using reverse-phase C18 column at $40^{\circ}C$ with $H_2O$ and acetonitrile (70:30, v/v) as an isocratic mobile phase at a flow rate of 1.0 mL/min and detection wavelength of UV 205 nm. This HPLC/UV analytical method showed good specificity and high linearity in the tested range of 0.03125-2.0mg/ml with excellent coefficient of determination ($R^2$) of 0.9999. The limit of detection and limit of quantification were $12.0{\mu}g/mL$ and $36.5{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 0.2% and 0.1%, respectively. These results indicate that the established HPLC/UV analytical method is very simple, specific, precise, accurate, and reproducible and thus can be useful for the quantitative analysis of HE as a functional anti-hypertensive compound in AE extract.

Determination of 10${\alpha}$-Methoxy-9,10-dihydrolysergol (MDL), Main Metabolite of Nicergoline, in Human Plasma by HPLC-MS and Applicability to Oral Bioavailability in Korean Healthy Male Volunteers (HPLC-MS를 이용한 생체시료 중 니세르골린의 주대사체인 10${\alpha}$-Methoxy-9,10-dihydrolysergol(MDL)의 분석 및 이를 이용한 한국인 성인 남성에 대한 생체이용률 응용)

  • Lim, Hyon-Kyun;Yoo, Sun-Dong;Kim, Kyeong-Ho;Han, Sang-Beom;Youm, Jeong-Rok
    • YAKHAK HOEJI
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    • v.51 no.2
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    • pp.133-139
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    • 2007
  • A simple and sensitive HPLC-MS method for quantitation of 10${\alpha}$-methoxy-9,10-dihydrolysergol (MDL), the main metabolite of nicergoline, in human plasma was developed and the bioavailability parameters of MDL was assessed in Korean healthy male volunteers. Clomipramine was used as an internal standard. MDL and internal standard in plasma sample were extracted using ethyl acetate. A centrifuged upper layer was then evaporated and reconstituted with mobile phase of 10 mM ammonium acetate-acetonitrile (10 : 90, v/v). The reconstituted samples were injected into a Zorbax SB-C8 column (2.1${\times}$150 mm,5 ${\mu}$m) at a flow-rate of 0.3 ml/min. Using MS with selected ion monitoring (SIM) mode, MDL and clomipramine were detected without severe interference from human plasma matrix. MDL produced a protonated molecular ion ([M+H]$^+$) at m/z 287. Internal standard produced a protonated molecular ion ([M+H]$^+$) at m/z 315. A linear relationship for MDL was found in the range of 2.5${\sim}$100 ng/ml. The lower limit of quantitation (LLOQ) was 2.5 ng/ml with acceptable precision and accuracy. The intra- and inter-day validation for all coefficients of variation (R.S.D.%) were found less than 15%. Main pharmacokinetic parameters of 30 mg of nicergoline were revealed as follows: AUC$_t$ 321.1${\pm}$64.5 ng${\cdot}$hr/ml, C$_{max}$, 51.2${\pm}$25.3 ng/ml, T$_{max}$ 3.6${\pm}$1.5 hr, K$_{el}$ 0.12${\pm}$0.07 hr$^{-1}$ and t$_{1/2}$ 7.6${\pm}$3.4 hr. Inter subject variations and race differences were shown in comparison with the published data in the literature.

Modelling the Effects of Temperature and Photoperiod on Phenology and Leaf Appearance in Chrysanthemum (온도와 일장에 따른 국화의 식물계절과 출엽 예측 모델 개발)

  • Seo, Beom-Seok;Pak, Ha-Seung;Lee, Kyu-Jong;Choi, Doug-Hwan;Lee, Byun-Woo
    • Korean Journal of Agricultural and Forest Meteorology
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    • v.18 no.4
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    • pp.253-263
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    • 2016
  • Chrysanthemum production would benefit from crop growth simulations, which would support decision-making in crop management. Chrysanthemum is a typical short day plant of which floral initiation and development is sensitive to photoperiod. We developed a model to predict phenological development and leaf appearance of chrysanthemum (cv. Baekseon) using daylength (including civil twilight period), air temperature, and management options like light interruption and ethylene treatment as predictor variables. Chrysanthemum development stage (DVS) was divided into juvenile (DVS=1.0), juvenile to budding (DVS=1.33), and budding to flowering (DVS=2.0) phases for which different strategies and variables were used to predict the development toward the end of each phenophase. The juvenile phase was assumed to be completed at a certain leaf number which was estimated as 15.5 and increased by ethylene application to the mother plant before cutting and the transplanted plant after cutting. After juvenile phase, development rate (DVR) before budding and flowering were calculated from temperature and day length response functions, and budding and flowering were completed when the integrated DVR reached 1.33 and 2.0, respectively. In addition the model assumed that leaf appearance terminates just before budding. This model predicted budding date, flowering date, and leaf appearance with acceptable accuracy and precision not only for the calibration data set but also for the validation data set which are independent of the calibration data set.