• Title/Summary/Keyword: Relative precision

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Analysis of coenzyme Q 1O in dietary supplement by HPLC (HPLC를 이용한 건강기능식품 중 코엔자임 Q10 성분 분석)

  • No, Ki-Mi;Leem, Dong-Gil;Kim, Mi-Gyeong;Park, Kyoung-Sik;Yoon, Tae-Hyung;Hong, Jin;Park, Sun-Young;Jeong, Ja-Young
    • Journal of Food Hygiene and Safety
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    • v.26 no.1
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    • pp.12-15
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    • 2011
  • A method based on high-performance liquid chromatography (HPLC) with ultraviolet detection has been developed to quantify coenzyme Q10 (CoQ10) in raw materials and dietary supplements. Single-laboratory validation has been performed on the method to determine linearity, selectivity, accuracy, limits of quantification (LOQ) and repeatability for CoQ10. An excellent linearity (r=0.999) was observed for CoQ10 in the concentration range $15.625{\sim}500\;{\mu}g/ml$ in dietary supplement. Observed recovery of CoQ10 was found to be between 98.33 and 99.38%. LOQ was found to be $250\;{\mu}g/ml$ Repeatability precision for CoQ10 was between 0.15 and 0.21% relative standard deviation (RSD). Further, limited studies showed that some adulterants and degraded material could be satisfactorily separated from CoQ10 and identified.

Pharmacodynamic Modeling of Vincristine in Lymphoma Patients (림프종 환자에서 회귀모형을 이용한 vincristine의 약물 용량 예측 인자 및 부작용 모델 연구)

  • Seo, Jeong-Won;Kim, Dong-Hyun;Yun, Jin-Sang;Kim, Seon-Hwa;Choi, Bo-Yoon;Oh, Jung-Mi;Kwon, Kwang-Il
    • Korean Journal of Clinical Pharmacy
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    • v.21 no.2
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    • pp.145-155
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    • 2011
  • The objective of this study was to determine whether any pretreatment parameters were associated with pharmacological effect or toxicity parameters after vincristine administration and to describe a mathematical model, which explains the interpatient pharmacodynamic variability. The relationship between patient characteristics and vincristine dose and hematological toxicity were evaluated. 68 pediatric and adolescence patients and 107 adults with acute lymphoblastic leukemia were treated with vincristine $1.5mg/m^2/day$ IV and other anticancer drugs as scheduled. Complete blood counts and other blood test results were obtained. The input variables were age, gender, weight, lean body weight (LBW), height, body surface area, vincristine dose and total vincristine dose. The outcome measures were nadir values (white blood cells, absolute neutrophil counts, hemoglobin, and platelets); the absolute decrease, relative decrease, and survival fraction of blood cells. Polynomial regression analysis was carried out to determine the other significant covariates. The variability of $WBC_{nadir}$ was modeled with good precision and accuracy with a two-covariate model. This model should be validated and improved on with further clinical data. We believe that such pharmacodynamic modeling should be explored further to determine its performance and clinical relevance compared with modeling using pharmacokinetic parameter.

Development and Evaluation of a Badge-type Passive Sampler for the Measurement of Short-term Nitrogen Dioxide in Ambient Air (대기 중 이산화질소의 단기 측정을 위한 뱃지형 passive sampler의 개발 및 평가)

  • Kim Sun Kyu;Yim Bong Been;Jung Eui Suk;Kim Sun Tae
    • Journal of Korean Society for Atmospheric Environment
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    • v.22 no.1
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    • pp.117-126
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    • 2006
  • The purpose of this study is to develop a badge-type passive sampler for the measurement of short-term nitrogen dioxide and to evaluate its performance. The principle of the method is a colorimetric reaction of nitrogen dioxide with sulfanilic acid, N-1-naphthylethylendiamine, and phosphoric acid. First, it has been shown that the filter paper should be rinsed with ultrapure water and ultrasound, and then dried in a vacuumed desiccator. The concentration and volume of absorption reagent (triethanolamine) were $20\%$ and 100 ${\mu}L$, respectively. The extraction time was determined as 60 min. Second, duplicate measurements (n= 116) were carried out for evaluating the precision of the passive sampler. The relative error and the correlation coefficient between duplicates are $3.4\pm 3.0\%$ and 0.994, respectively. In addition, the $95\%$ confidence interval of intraclass correlation coefficient and the estimated value are 0.992$\sim$0.996 and 0.994, respectively. Third, a paired t-test was carried out for evaluating the accuracy of the passive sampler (n=40). In the result of the test, the $95\%$ confidence interval of the difference was -1.710 ppb <$\gamma$< 0.788 ppb. Finally, the average concentration of blanks, measurement detection limit, limit of detection, and limit of quantification are $2.4\pm 0.4$ ppb, 104 ppb, 3.8 ppb, and 7.0 ppb, respectively.

Understanding Complex Design Features via Design Effect Models (설계효과모형을 통한 설계요소의 유용성 이해)

  • Park, Inho
    • The Korean Journal of Applied Statistics
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    • v.28 no.6
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    • pp.1217-1225
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    • 2015
  • Survey research, data is commonly collected through a sample design with complex design features that allow the relative efficiency on the precision of an estimator to be measured using the concept of the design effect compared to simple random sampling as a reference design. This concept is most useful when the design effect can be expressed as a function of various design features. We propose a design effect formula suitable under a stratified multistage sampling by generalizing Gabler et al. (1999, 2006)'s approaches for multistage sampling. Its use can either guide improvement in the design efficiency when in design stage or enable the evaluation of the adopted design features afterwards.

Simultaneous Quantification of Three Marker Compounds in Samultang by HPLC/DAD (HPLC-DAD를 이용한 사물탕 중 3종 성분의 동시분석법 확립)

  • Won, Jin-Bae;Ma, Jin-Yeul;Lee, Jae-Hoon;Ma, Choong-Je
    • Korean Journal of Pharmacognosy
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    • v.40 no.4
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    • pp.298-302
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    • 2009
  • Samultang is one of traditional medicine composed of Paeonia lactiflora, Angelica gigas, Rehmannia glutinosa and Cnidium officinale. To develop simultaneous determination of paeoniflorin, decursin and 5-HMF in Samultang, a high performance liquid chromatography with diode array detector was used. To separate three marker components, Dionex $C_{18}$ column (5 ${\mu}m$, 120 ${\AA}$, 4.6 mm${\times}$150 mm) was used with a gradient elution system of water and methanol. UV wavelength of detector set at 230 nm and 280 nm. This method was validated by linearity, precision test and recovery test. Calibration curves of three standard components were showed good linear regression ($R^2$>0.9973). LOD and LOQ ranged from 0.08 ${\mu}g$/ml to 0.38 ${\mu}g$/ml and 0.25 ${\mu}g$/ml to 1.16 ${\mu}g$/ml, respectively. The relative standard deviations (RSDs) of data of the inter-day and intra-day experiments were less than 0.54% and 0.89%, respectively. The measured results of recovery test were varied from 93.36 to 107.79 with RSD values 0.01~1.45%. The established method was applied for separation of bio-conversion Samultang sample and compared with control sample.

Validation of an HPLC Analytical Method for Determination of Biogenic Amines in Agricultural Products and Monitoring of Biogenic Amines in Korean Fermented Agricultural Products

  • Yoon, Hyeock;Park, Jung Hyuck;Choi, Ari;Hwang, Han-Joon;Mah, Jae-Hyung
    • Toxicological Research
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    • v.31 no.3
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    • pp.299-305
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    • 2015
  • An HPLC analytical method was validated for the quantitative determination of biogenic amines in agricultural products. Four agricultural foods, including apple juice, Juk, corn oil and peanut butter, were selected as food matrices based on their water and fat contents (i.e., non-fatty liquid, non-fatty solid, fatty liquid and fatty solid, respectively). The precision, accuracy, recovery, limit of detection (LOD) and quantification (LOQ) were determined to test the validity of an HPLC procedure for the determination of biogenic amines, including tryptamine, ${\beta}$-phenylethylamine, putrescine, cadaverine, histamine, tyramine, spermidine and spermine, in each matrix. The LODs and LOQs for the biogenic amines were within the range of 0.01~0.10 mg/kg and 0.02~0.31 mg/kg, respectively. The relative standard deviation (RSD) of intraday for biogenic amine concentrations ranged from 1.86 to 5.95%, whereas the RSD of interday ranged from 2.08 to 5.96%. Of the matrices spiked with biogenic amines, corn oil with tyramine and Juk with putrescine exhibited the least accuracy of 84.85% and recovery rate of 89.63%, respectively, at the lowest concentration (10 mg/kg). Therefore, the validation results fulfilled AOAC criteria and recommendations. Subsequently, the method was applied to the analysis of biogenic amines in fermented agricultural products for a total dietary survey in Korea. Although the results revealed that Korean traditional soy sauce and Doenjang contained relatively high levels of histamine, the amounts are of no concern if these fermented agricultural products serve as condiments.

Establishing of a rapid analytical method on uranium isotopic ratios for the environmental monitoring around nuclear facilities (원자력 시설 주변 환경 감시를 위한 토양 중 우라늄 동위원소 신속 분석법 확립)

  • Park, Ji-Young;Lim, Jong-Myoung;Lee, Hyun-Woo;Lee, Wanno
    • Analytical Science and Technology
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    • v.31 no.3
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    • pp.134-142
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    • 2018
  • The uranium isotopic ratio in environmental samples around nuclear facilities is important because it reveals information regarding illegal activities or anthropogenic pollution. Determination of uranium isotopes, however, is a challenging task requiring much labor and time because of the complex separation procedures and lengthy process. In this study, a rapid determination method for uranium isotopes in environmental samples was developed using. The sample was completely decomposed using the alkali fusion method. The separation procedure using extraction chromatography (UTEVA) was simplified in a single step without any further removal process for Si and major matrix elements. The established method can be completed within 3 h from sample dissolution to ICP-MS measurement. Most matrix elements and uranium isotopes in the soil samples were well separated and purified. Five types of were used to assess the method's accuracy and precision for a rapid uranium analysis method. The analytical accuracy for all CRM samples ranged from 95.1 % to 97.8 %, and the relative standard deviation was below 3.9 %. From the analytical results, one may draw conclusions that the evaluated method for uranium isotopes using alkali-fusion, the extraction chromatography process, and ICP-MS measurements is fast and fairly reliable owing to its recovering efficiencies. Thus, it is expected that the evaluated method can contribute to the improvement of environmental monitoring ability.

A Study on the Utility of Relevance/Non-relevance Information in Homogeneous Documents (유사문헌집단에서 적합/부적합정보의 유용성에 관한 연구)

  • Moon, Sung-Been
    • Journal of the Korean Society for information Management
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    • v.32 no.3
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    • pp.277-293
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    • 2015
  • This study examined the relative retrieval effectiveness after relevance feedback between two systems (Title/Abstract and Full-text) using four different sets of relevance judgment. Four relevance levels (not relevant, marginally relevant, relevant, highly relevant) are also used, each of which is determined by referees giving a relevance score to documents. This study also investigated how much the average precision was improved after relevance feedback when "marginally relevant" documents are included in the relevant class with the Title/Abstract system, and with the Full-text retrieval system as well. It is found that the Title/Abstract system benefited from relevance feedback with the marginally relevant documents. In case of the Title/Abstract system, the higher percentage of improvement was consistently obtained when including the marginally relevant documents in the relevance class, however the result was vice versa in case of the Full-text retrieval system. It implied that the marginally relevant documents in the relevant class had caused noises in the Full-text retrieval system.

Determination of Glutathione in Biological Samples by Ion-pairing HPLC/FLD (이온쌍 HPLC/FLD를 이용한 생체 시료중의 Glutathione 농도 분석)

  • Yoo, Jeong-Yeon;Lee, Kyoung-Ok;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.12 no.1
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    • pp.28-33
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    • 1999
  • Glutathione(GSH) in biological samples was determined by high performance liquid chromatographic(HPLC) method with fluorescence detector(FLD) after monobromobimane(MBB) or 4-fluoro-7-sulfobenzofurazan(SBD-F) derivatization. The detection limit of $0.03{\mu}g/mL$ was obtained after MBB derivatization, derivative of MBB was about 200 times more sensitive than that of SBD-F. N-acetylcysteine was used as internal standard and tetrabutylammonium ion as counter ion for better separation. The determination by ion-pairing chromatography after MBB derivatization was characterized by linearity in the range between $0.08{\sim}8.33{\mu}g/mL$ with a good correlation coefficient of 0.998. By precision test appeared relative standard deviation at less than 5% at three different concentrations. This method can be used for the analysis of GSH in plasma and tissue.

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Simultaneous determination of fluorometholone and tetrahydrozoline hydrochloride in ophthalmic suspension by HPLC

  • Pham, Thuy-Vy;Mai, Xuan-Lan;Song, Ha-Ram;Ahn, Soo-Bin;Cha, Min-Jeong;Kang, Jong-Seong;Woo, Mi Hee;Na, Dong-Hee;Chun, In-Koo;Kim, Kyeong Ho
    • Analytical Science and Technology
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    • v.31 no.2
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    • pp.88-95
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    • 2018
  • A simple, sensitive, and selective high-performance liquid chromatography (HPLC) method was developed and validated for the simultaneous quantification of fluorometholone (FLU) and tetrahydrozoline hydrochloride (THZ) in combined ophthalmic formulations. The effects of several factors, including detection wavelength, buffer pH, buffer concentration, and organic solvent concentration, on the performance of the method were investigated. The performance of the developed method was validated in accordance with the requirements of the International Conference on Harmonization. The linearity of the calibration curves in the desired concentration range was high for both FLU and THZ ($r^2=0.9999$). The accuracy and precision of the method were determined by a recovery study at analyte concentrations of 80 %, 100 %, and 120 %. The recovery was 99.60-100.17 % for both analytes, with a relative standard deviation less than 1.0 % at any concentration level. The validated results indicate that the new HPLC method could be successfully applied for the simultaneous determination of FLU and THZ in ophthalmic suspensions.