• Title/Summary/Keyword: 표준측정법

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Development and Validation of the Determination of Sorafenib in Human Plasma using Tandem Mass Spectrometry Coupled with Liquid Chromatography (고속액체크로마토그래피 텐덤질량분석기법을 이용한 사람 혈장 내 소라페닙 농도분석법의 개발 및 검정)

  • Park, Daejin;Lee, Sunggon;Kim, Woomi
    • Journal of Life Science
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    • v.22 no.11
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    • pp.1456-1462
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    • 2012
  • Sorafenib is a multikinase inhibitor and an oral anticancer drug approved for the treatment of patients with advanced renal cell carcinoma and those with unresectable hepatocellular carcinoma. The purpose of this study was to develop an efficient method of the determination of sorafenib in human plasma using tandem mass spectrometry coupled with liquid chromatography (LC/MS/MS) and validate the method by the guidelines of the Korean Food and Drug Administration (KFDA). Plasma samples ($100{\mu}l$) were added with chlorantraniliprole as an internal standard and then mixed with the 0.1% formic acid-containing extraction solution composed of isopropyl alcohol and ethyl acetate (1:4, v/v). After centrifugation, the supernatant was concentrated at $45^{\circ}C$ under negative pressure and centrifugal force. The residue was reconstituted with a mobile phase and injected into the HPLC instrument using a reverse phase Waters XTerra$^{TM}$ C18 column (particle size $3.5{\mu}m$). Liquid chromatography was carried out within the run time of 5 min using a mobile phase composed of buffer (0.1% formic acid and 10 mM ammonium formate), methanol, and acetonitrile (1:6:3, v/v/v). The analytes were monitored by tandem mass spectrometry in the multiple reaction monitoring method programmed to detect sorafenib at 'm/z 465.2 ${\rightarrow}$ 252.5' and chlorantraniliprole at 'm/z 484.4 ${\rightarrow}$ 286.2' with positive electrospray ionization mode ($ES^+$). The result showed the proper linearity ($r^2$ > 0.99) over the range of 2,000-5,000 ng/ml with good accuracy (90.7-103.9%) and precision (less than 10%). The newly developed method using LC/MS/MS was validated by the guideline of KFDA and identified as more sensitive compared to the previous methods.

Improved Breast Irradiation Techniques Using Multistatic Fields or Three Dimensional Universal Compensators (Multistatic Field또는 3차원 공용보상체를 사용한 유방의 방사선 조사법의 평가)

  • Han Youngyih;Cho Jae Ho;Park Hee Chul;Chu Sung Sil;Suh Chang-Ok
    • Radiation Oncology Journal
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    • v.20 no.1
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    • pp.24-33
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    • 2002
  • Purpose : In order to improve dose homogeneity and to reduce acute toxicity in tangential whole breast radiotherapy, we evaluated two treatment techniques using multiple static fields or universal compensators. Materials and Methods : 1) Multistatic field technique : Using a three dimensional radiation treatment planning system, Adac Pinnacle 4.0, we accomplished a conventional wedged tangential plan. Examining the isodose distributions, a third field which blocked overdose regions was designed and an opposing field was created by using an automatic function of RTPS. Weighting of the beams was tuned until an ideal dose distribution was obtained. Another pair of beams were added when the dose homogeneity was not satisfactory. 2) Universal compensator technique : The breast shapes and sizes were obtained from the CT images of 20 patients who received whole breast radiation therapy at our institution. The data obtained were averaged and a pair of universal physical compensators were designed for the averaged data. DII (Dose Inhomogeneity Index : percentage volume of PTV outside $95\~105\%$ of the prescribed dose) $D_{max}$ (the maximum point dose in the PTV) and isodose distributions for each technique were compared. Results : The multistatic field technique was found to be superior to the conventional technique, reducing the mean value of DII by $14.6\%$ (p value<0.000) and the $D_{max}$ by $4.7\%$ (p value<0.000). The universal compensator was not significantly superior to the conventional technique since it decreased $D_{max}$ by $0.3\%$ (p value=0.867) and reduced DII by $3.7\%$ (p value=0.260). However, it decreased the value of DII by maximum $18\%$ when patients' breast shapes fitted in with the compensator geometry. Conclusion : The multistatic field technique is effective for improving dose homogeneity for whole breast radiation therapy and is applicable to all patients, whereas the use of universal compensators is effective only in patients whose breast shapes fit inwith the universal compensator geometry, and thus has limited applicability.

Recovery Trajectory in Tachycardia Induced Heart Failure Model (빈맥을 이용한 심부전 모델에서 회복궤도)

  • 오중환;박승일;원준호;김은기;이종국
    • Journal of Chest Surgery
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    • v.32 no.5
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    • pp.422-427
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    • 1999
  • Background: Tachycardia induced heart failure model would be the model of choice for the dilated cardiomyopathy. This more closely resembles the clinical syndrome and does not require major surgical trauma, myocardial ischemia and pharmacological or toxic depression of cardiac function. When heart failure is progressive, application of new surgical procedures to the faling heart is highly risky. It has been shown that recovery trajectory from heart failure is a new method in decreasing animal mortality. The purpose is to establish the control datas for recovery trajectory in the canine heart failure model. Material and Method: 21 mongrel dogs were studied at 4 stages(baseline, at the heart failure, 4 and 8 weeks after recovery). Heart failure was induced during 4 weeks of continuous rapid pacing using a pacemaker. Eight weeks of trajectory of recovery period was allowed. Indices of left ventricular function and dimension were measured every 2 weeks and the hemodynamics were measured by use of Swan-Ganz catheterization and thermodilution method every 4 weeks. Values were expressed as mean${\pm}$standard deviation. Result: 4(20%) dogs died due to heart failure. Left ventricular end-diastolic volume at the 4 stages were 40.8${\pm}$7.4, 82.1${\pm}$21.1, 59.9${\pm}$7.7 and 46.5${\pm}$6.5ml. Left ventricular end-systolic volume showed the same trend. Ejection fractions were 50.6${\pm}$4.1, 17.5${\pm}$5.8, 36.3${\pm}$7.3, and 41.5${\pm}$2.4%. Blood pressure and heart rate showed no significant changes. Pressures of central vein, right ventricle, pulmonary artery, and pulmonary capillary wedge showed significant increase during the heart failure period, normalizing at the end of recovery period. Stroke volumes were 21.5${\pm}$8.2, 12.3${\pm}$3.5, 17.9${\pm}$4.6, and 15.5${\pm}$3.4ml. Blood norepinephrine level was 133.3${\pm}$60.0pg/dL at the baseline and 479.4${\pm}$327.3pg/dL at the heart failure stage(p=0.008). Conclusion: Development of tachycardia induced heart failure model is of high priority due to ready availability and reasonable amenability to measurements. Recovery trajectory after cessation of tachycardia showed reduction of cardiac dilatation and heart function. Application of new surgical procedures during the recovery period could decrease animal mortality.

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Normative data of penile length in Korean newborns (한국인 신생아 음경 길이에 대한 연구)

  • Kim, Sang Yeob;Jun, Jae Sung;Lee, Sang Geel
    • Clinical and Experimental Pediatrics
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    • v.51 no.9
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    • pp.944-949
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    • 2008
  • Purpose : As modern society has became more open, interest in healthy internal and external growth has increased, including that pertaining to penile length in children. A micropenis is defined as one where penile length is more than 2 SD (standard deviation) below the mean, and it can be traced back to chromosome and endocrine disorders. The authors executed this study to suggest guidelines for the study of the micropenis and standard information for penile length in Korean newborns. Methods : The subjects of this study were 168 male infants between 37 and 42 weeks of gestational age, none of whom had any complications during pregnancy or birth; each had been born in Daegu Fatima Hospital between February and June 2007. Penile length was measured using conventional stretched penile length measurement (CPLM) and syringe methods. Results : Penile length was $3.02{\pm}0.25cm$ (F=36.467, $R^2=0.180$, P<0.001) when measured with CPLM, and $3.29{\pm}0.26cm$ (F=9.149, $R^2=0.052$, P<0.001) with the syringe method. There was no statistically significant difference in the penile length of newborn infants as a result of taking measurements with the two methods, and both methods showed significance at 0.631 in terms of Pearson's correlation coefficient, at the level of P=0.01. Conclusion : In this study, penile length tended to be longer when gestational age was longer, and a micropenis can be assumed to be one less than 2.5 cm using CPLM and less than 2.8 cm using the syringe method. In the case of a concealed penis, the syringe method is helpful. When a micropenis is assumed, close observation by outpatient department personnel, and additional endocrine and chromosome studies should be undertaken after sufficiently consulting the parents.

Methodological Comparison of the Quantification of Total Carbon and Organic Carbon in Marine Sediment (해양 퇴적물내 총탄소 및 유기탄소의 분석기법 고찰)

  • Kim, Kyeong-Hong;Son, Seung-Kyu;Son, Ju-Won;Ju, Se-Jong
    • Journal of the Korean Society for Marine Environment & Energy
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    • v.9 no.4
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    • pp.235-242
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    • 2006
  • The precise estimation of total and organic carbon contents in sediments is fundamental to understand the benthic environment. To test the precision and accuracy of CHN analyzer and the procedure to quantify total and organic carbon contents(using in-situ acidification with sulfurous acid($H_2SO_3$)) in the sediment, the reference material s such as Acetanilide($C_8H_9NO$), Sulfanilammide($C_6H_8N_2O_2S$), and BCSS-1(standard estuary sediment) were used. The results indicate that CHN analyzer to quantify carbon and nitrogen content has high precision(percent error=3.29%) and accuracy(relative standard deviation=1.26%). Additionally, we conducted the instrumental comparison of carbon values analyzed using CHN analyzer and Coulometeric Carbon Analyzer. Total carbon contents measured from two different instruments were highly correlated($R^2=0.9993$, n=84, p<0.0001) with a linear relationship and show no significant differences(paired t-test, p=0.0003). The organic carbon contents from two instruments also showed the similar results with a significant linear relationship($R^2=0.8867$, n=84, p<0.0001) and no significant differences(paired t-test, p<0.0001). Although it is possible to overestimate organic carbon contents for some sediment types having high inorganic carbon contents(such as calcareous ooze) due to procedural and analytical errors, analysis of organic carbon contents in sediments using CHN Analyzer and current procedures seems to provide the best estimates. Therefore, we recommend that this method can be applied to measure the carbon content in normal any sediment samples and are considered to be one of the best procedure far routine analysis of total and organic carbon.

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Simultaneous Separation and Determination of $^{l4}C\;and\;^3H$ in Spent Resins from PWR Nuclear Power Plants (가압경수로형 원전에서 발생된 폐수지의 $^{14}C$$^3H$ 동시 분리 및 측정)

  • Park, Soon-Dal;Kim, Jung-Suck;Kim, Jong-Goo;Han, Sun-Ho;Jee, Kwang-Yong
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.5 no.3
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    • pp.179-188
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    • 2007
  • In this work $^{14}C\;and\;^3H$ distribution characteristics of spent resins from nuclear power plants(NPPs), pressurized water reactors(PWRs), was investigated. It was found that the recovery percent of $^{14}C$ by the wet oxidation-acid stripping was $81%{\sim}100%$ for the added activity range of $^{14}C,\;0.72\;Bq{\sim}460\;Bq$, and it was not affected by the kinds of stripping acids, 3N-HCl, $3\;N-HNO_3\;and\;3\;N-H_2SO_4$. And the recovery percent of $^3H$ by distillation using the same apparatus was $81%{\sim}101%$ for the added activity range of $^3H,\;0.60\;Bq{\sim}435\;Bq$. Among the tested stripping acids, 3\;N-HCl, $3\;N-HNO_3\;and\;3\;N-H_2SO_4$, only the trapped $^3H$ solution by distillation in $3\;N-H_2SO_4$ was compatible with the 3H scintillator, Ultimagold XR. Neither of the $^{14}C\;and\;^3H$ trapping solutions from the spent ion exchange resin samples by the wet oxidation-3 $N-H_2SO_4$ stripping contained gamma nuclides. However, some gamma nuclides, $^{60}Co,\;^{134}Cs,\;^{137}Cs\;and\;^{54}Mn$, were found in the trapped $^3H$ solutions of the spent resins by the wet oxidation-3 N-HCl stripping. It was the same for the $^3H$ trapping solutions of the spent resins by Sample Oxidizer(PACKARD MODEL 307). Meanwhile only two nuclides, $^{134}Cs,\;and\;^{134}Cs$, were found in the $^{14}C$ trapping solutions of the spent resins by Sample Oxidizer(PACKARD MODEL 307). It was found that most of the $^{14}C$ in the spent resins existed as inorganic carbon form, more than about 70% of the total $^{14}C$ content. Among the analyzed 30 spent ion exchange resin samples, the average concentration of $^{14}C$ and $^3C$ for the high radioactive samples, 8 samples, was $19000\;Bq/g{\pm}41000\;Bq/g,\;670\;Bq/g{\pm}460\;Bq/g$ and that for the low radioactive samples, 22 samples, was $4.2\;Bq/g{\pm}4.3\;Bq/g,\;6.0\;Bq/g{\pm}5.3\;Bq/g$, respectively. And the average $^{14}C/^3H$ ratio for the high radioactive samples, was higher, 28, than that of low radioactive samples, 0.70. Some linear relationship trend was found between the activity concentrations of $^{14}C\;and\;^3H$.

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Quantitative Analysis for Components of Epimedium koreanum (음양곽 주성분의 정량분석)

  • Han, Yong-Nam;Hwang, Keum-Hee;Lee, Mie-Soon
    • Korean Journal of Food Science and Technology
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    • v.28 no.4
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    • pp.616-623
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    • 1996
  • Eum Yang Kwak, the aerial part of Epimedium koreanum, is widely used as a folk medicine for stimulant in man, tonic, and hypotensive purpose. The plant contains icariin (a specific flavonoid), magnoflorine (an alkaloid) and tannin, but their contents are not known until now. In this paper, a quantitative analysis method for them was developed. Determination of icariin and magnoflorine was successfully achived by high performance liquid chromatography equipped with a UV detector in the ranges of $0.1{\sim}0.4\;mg$ and $0.002{\sim}0.1\;mg\;per\;ml$ sample, respectively. Extraction of the plant was carried out with water or 50% ethanol using different decocting temperatures and times. Icariin was well extracted either by water ($100^{\circ}C$, 3hr) or 50% ethanol ($85^{\circ}C$, 1hr), and its content in the plant was measured to be 0.94%. On the other hand, magnoflorine was fully extracted by 50% ethanol ($85^{\circ}C$, 1hr), and its content was determined to be 0.16%. Therefore, decoction of the medicinal plant with water at $100^{\circ}C$ for 3hr turned out to be recommendable for the best extraction.

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Prediction on the Quality of Total Mixed Ration for Dairy Cows by Near Infrared Reflectance Spectroscopy (근적외선 분광법에 의한 국내 축우용 TMR의 성분추정)

  • Ki, Kwang-Seok;Kim, Sang-Bum;Lee, Hyun-June;Yang, Seung-Hak;Lee, Jae-Sik;Jin, Ze-Lin;Kim, Hyeon-Shup;Jeo, Joon-Mo;Koo, Jae-Yeon;Cho, Jong-Ku
    • Journal of The Korean Society of Grassland and Forage Science
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    • v.29 no.3
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    • pp.253-262
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    • 2009
  • The present study was conducted to develop a rapid and accurate method of evaluating chemical composition of total mixed ration (TMR) for dairy cows using near infrared reflectance spectroscopy (NIRS). A total of 253 TMR samples were collected from TMR manufacturers and dairy farms in Korea. Prior to NIR analysis, TMR samples were dried at $65^{\circ}C$ for 48 hour and then ground to 2 mm size. The samples were scanned at 2 nm interval over the wavelength range of 400-2500 nm on a FOSS-NIR Systems Model 6500. The values obtained by NIR analysis and conventional chemical methods were compared. Generally, the relationship between chemical analysis and NIR analysis was linear: $R^2$ and standard error of calibration (SEC) were 0.701 (SEC 0.407), 0.965 (SEC 0.315), 0.796 (SEC 0.406), 0.889 (SEC 0.987), 0.894 (SEC 0.311), 0.933 (SEC 0.885) and 0.889 (SEC 1.490) for moisture, crude protein, ether extract, crude fiber, crude ash, acid detergent fiber (ADF) and neutral detergent fiber (NDF), respectively. In addition, the standard error of prediction (SEP) value was 0.371, 0.290, 0.321, 0.380, 0.960, 0.859 and 1.446 for moisture, crude protein, ether extract, crude fiber, crude ash, ADF and NDF, respectively. The results of the present study showed that the NIR analysis for unknown TMR samples would be relatively accurate. Use of the developed NIR calibration curve can obtain fast and reliable data on chemical composition of TMR. Collection and analysis of more TMR samples will increase accuracy and precision of NIR analysis to TMR.

Method Validation for the Determination of Eleutherosides and β-Glucan in Acanthopanax koreanum (탐라오가피의 Eleutheroside B, E 및 β-Glucan 함량 분석 및 분석법 검증)

  • Kim, Young-Hyun;Bae, Da-Bin;Park, Sun-Ok;Lee, Sang-Jong;Cho, Ok-Hyun;Lee, Ok-Hwan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.42 no.9
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    • pp.1419-1425
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    • 2013
  • The aim of this study was to investigate the method validation for the determination of eleutherosides (B and E) and ${\beta}$-glucan in Acanthopanax (A.) koreanum. This medicinal plant reportedly mainly included eleutherosides which exhibit the pharmacological effects, and ${\beta}$-glucan substantially enhances the function of the immune system by activating macrophages. The specificity, linearity, precision, accuracy, limit of detection (LOD, S/N=3), and limit of quantification (LOQ, S/N=10) were measured by HPLC and enzymatic methods. Our results showed that the coefficient of calibration correlation ($R^2$) for eleutheroside B and E were 0.9997 and 0.9999, respectively. The limits of detection (LOD) for eleutheroside B and E were $0.050{\mu}g/mL$ and $0.025{\mu}g/mL$, respectively. The recovery rate of eleutheroside B and E were revealed in the high range of 100.66~110.04% and 94.26~111.62%, respectively. The inter-day precision of eleutheroside B and E in the root and stem in A. koreanum were 1.4~5.0% and 1.1~2.5%, respectively. The intra-day precision of eleutheroside B and E in the root and stem in A. koreanum were 2.8~2.9% and 0.4~1.1%, respectively. Furthermore, the inter-day and intra-day precision of ${\beta}$-glucan in the stem, leaf, and fruit of A. koreanum were 1.32~5.67% and 8.01~11.76%, respectively. In conclusion, the methods were validated for the detection of eleutherosides and ${\beta}$-glucan in A. koreanum.

Normative blood pressure references for Korean children and adolescents (한국 소아 청소년 정상 혈압 참고치)

  • Lee, Chong Guk;Moon, Jin Soo;Choi, Joong-Myung;Nam, Chung Mo;Lee, Soon Young;Oh, Kyungwon;Kim, Young Taek
    • Clinical and Experimental Pediatrics
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    • v.51 no.1
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    • pp.33-41
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    • 2008
  • Purpose : It is now understood that blood pressure (BP) measurement in the routine pediatric examination is very important because of the relevance of childhood BP to pediatric health care and the development of adult essential hypertension. There hasn't been a reference table of BP for Korean children and adolescents up to now. This study was to make normative BP references and to provide criteria of hypertension for Korean children and adolescents. Methods : BP measurements were done on 57,433 Koean children and adolescents (male: 29,443, female: 27,990), aged 7 to 20 years, in 2005. Heights and weights were measured simultaneously. Oscillometric devices, Dinamap Procare 200 (GE Inc., Milwaukee, Wi, USA), were used for the measurements. BPs were measured 2 times and mean levels were gathered for the analysis. Outliers of 2,373 subjects with overweight per height, over +3SD, were excluded for the analysis. For the BP centiles adjusted by sex, age and height, fixed modified LMS method which was adopted from the mixed effect model of 2004 Task Force in NHLBI (USA) was used. Results : Normative BP tables for Korean children and adolescents adjusted for height percentiles (5th, 10th, 25th, 50th, 75th, 90th, 95th), gender (male, female) and age(7 to 18 years) were completed. Height centiles of Korean children and adolescents are available from Korean Center for Disease Control and Prevention homepage, http://www.cdc.go.kr/webcdc/. Criteria of hypertension (95th, 99th percentile) and normal range of BP (50th, 90th) adjusted for height percentiles, age and gender were made. Conclusion : This is the first study to make normative BP tables and define hypertension for the Korean children and adolescents. Reliability and accuracy of Dinamap Procare 200 oscillometer for BP measurements remains debatable.