• 제목/요약/키워드: Column quantification

검색결과 318건 처리시간 0.028초

캐필러리 컬럼 종류에 따른 다이옥신 이성체 분리능과 정량 특성 변화 (Quantification and Resolution of Dioxins on Capillary Columns)

  • 김종국;박진수;김경심;이근희;김신조
    • 분석과학
    • /
    • 제15권1호
    • /
    • pp.43-53
    • /
    • 2002
  • 본 연구에서는 다이옥신 분석에 일반적으로 사용되고 있는 SP-2331, DB-5, DB-17, DB-DIOXIN 컬럼을 이용하여 소각로 배가스, 소각재, 대기, 토양, 어류 등을 대상으로 17RO 2,3,7,8-치환 이성체에 대한 분리능과 다이옥신 농도의 정량특성 변화를 검토하였다. 컬럼 종류에 따른 각시료별 정량 값 차이는 소각로 배가스, 토양, 소각재, 대기 그리고 어류 순으로 나타났다. 동일 시료에 대한 각 컬럼의 정량값은 DB-5가 가장 높은 농도를 나타냈으며, DB-17과 DB-DIOXIN 그리고 SP-2331 순으로 나타났다. SP-2331 컬럼을 기준으로 DB-5 컬럼은 2,3,7,8-TCDF를 최고 10배까지 높게 정량하는 것으로 나타났으며, DB-17 컬럼은 1,2,3,6,7,8-HxCDF가 상대적으로 2~3배정도 과대평가되었다. 또한 DB-DIOXIN 컬럼에서는 1,2,3,7,8-PeCDD가 상대적으로 1.5~2배 과대 평가하는 것으로 나타나 각각 컬럼에 따라 특정 이성체를 상대적으로 과대 평가하는 것으로 나타났다.

진동수주형 파력발전 시스템의 디지털 트윈 적용을 위한 불확실성 정량화 및 성능 신뢰구간 추정 연구 (A Study on Uncertainty Quantification and Performance Confidence Interval Estimation for Application to Digital Twin of Oscillating Water Column Type Wave Power Generator System)

  • 김태균;조수길;오재원;이태희
    • 한국산업융합학회 논문집
    • /
    • 제26권3호
    • /
    • pp.401-409
    • /
    • 2023
  • Oscillating water column (OWC) type wave power generator system is a power generation system that uses wave energy, a sustainable and renewable energy source. Irregular cycles and wave heights act as factors that make it difficult to secure generation efficiency of the wave power generator system. Recently, research for improving power generation efficiency is being conducted by applying digital twin technology to OWC type wave energy converter system. However, digital twin using sensor data can predict erroneous performance due to uncertainty in the sensor data. Therefore, this study proposes an uncertainty analysis method for sensor data which is used in digital twin to secure the reliability of digital twin prediction results. Uncertainty quantification considering sensor data characteristics and future uncertainty information according to uncertainty propagation were derived mathematically, and confidence interval estimation was performed based on the proposed method.

Quantification Plots for Several Sets of Variables

  • Park, Mira;Huh, Myung-Hoe
    • Journal of the Korean Statistical Society
    • /
    • 제25권4호
    • /
    • pp.589-601
    • /
    • 1996
  • Geometric approach to extend the classical two-set theory of canonical correlation analysis to three or more sets is considered. It provides statistical graphs to represent the data in a low dimensional space. Procedures are developed for computing the canonical variables and the corresponding properties are investigated. The solution is equivalent to that of the usual problem in the case of two sets. Goodness-of-fit of the proposed plots is studied and a numerical example is included.

  • PDF

High Speed Separation of PFCs in Human Serum by C18-Monolithic Column Liquid Chromatography-Tandem Mass Spectrometry

  • Lee, Won-Woong;Lee, Sun-Young;Yu, Se Mi;Hong, Jongki
    • Bulletin of the Korean Chemical Society
    • /
    • 제33권11호
    • /
    • pp.3727-3734
    • /
    • 2012
  • An analytical method has been developed for the rapid determination of perfluorinated compounds (PFCs) in human serum samples. The extraction and purification of PFCs from human serum were performed by the modified method of previous report. Ten PFCs were rapidly separated within 3.3 min by C18-monolithic column liquid chromatography (LC) and detected by electrospray ionization (ESI) tandem mass spectrometry (MS/MS) in negative ion mode. The runtime of PFCs on monolithic column LC was up to 4-fold faster than that on conventional column LC. The effect of triethylamine (TEA) to the mobile phase has investigated on the overall MS detection sensitivity of PFCs in ESI ionization. Quantification was performed by LC-MS/MS in multiple-ion reaction monitoring (MRM) mode, using $^{13}C$-labeled internal standards. Method validation was performed to determine recovery, linearity, precision, and limits of quantification, followed by, the analysis of a standard reference material (SRM 1957 from NIST). The overall recoveries ranged between 81.5 and 106.3% with RSDs of 3.4 to 16.2% for the entire procedure. The calibration range extended from 0.33 to 50 $ng\;mL^{-1}$, with a correlation coefficient ($R^2$) greater than 0.995 and the limits of quantification with 0.08 to 0.46 $ng\;mL^{-1}$. This approach can be used for rapid and sensitive quantitative analysis of 10 PFCs in human serum with high performance and accuracy.

Determination of Terbutaline Enantiomers in Human Plasma by Coupled Achiral-Chiral High Performance Liquid Chromatography

  • Kim, Kyeong-Ho;Kim, Hyun-Ju;Hong, Seon-Pyo;Shin, Sang-Deok
    • Archives of Pharmacal Research
    • /
    • 제23권5호
    • /
    • pp.441-445
    • /
    • 2000
  • Achiral-chiral column switching HPLC assay was developed to allow the separation and quantification of the enantiomers of terbutaline in human plasma by means of fluorescence detection. Plasma samples were prepared by solid-phase extraction with sep-pak silica, followed by HPLC assay. The enantiomers of terbutaline and the internal standard were separated from the biological matrix on a silica column, and the two enantiomers were resolved and quantified on a Sumichiral OA-4900 column. The two columns were connected by a switching valve equipped with silica trap column, The trap column was used to concentrate the terbutaline in the eluent from the achiral column before back flushing onto the chiral phase. For each enantiomers, the assay was linear between 2.5-125 ng/$m\ell$ (r=0.9999) and detection limit was 1.0 ng/$m\ell$ .

  • PDF

Dual Capillary Column System for the Qualitative Gas Chromatography: 2. Comparison between Splitless and On-Column Injection Modes

  • Kim, Kyoung-Rae;Kim, Jung-Han;Park, Hyoung-Kook;Oh, Chang-Hwan
    • Bulletin of the Korean Chemical Society
    • /
    • 제14권2호
    • /
    • pp.250-255
    • /
    • 1993
  • A dual capillary column system is described for the simultaneous analysis of a given sample and measurement of retention index (RI) and area ratio (AR) values of each peak on two capillary columns of different polarity, DB-5 & DB-1701 from a single injection. Both capillary columns were connected to either a splitless injector or an on-column injector via a deactivated fused-silica capillary tubing of 1 m length and a 'Y' splitter. Both injection modes allowed to measure RI and AR values with high reproducibility (<0.01% RSD) and high accuracy (<10% RE), respectively with the exception that the trace and high boiling solutes required the on-column mode for the accurate quantification and AR comparison. When the dual capillary column system in on-column injection mode was applied to the blind samples containing organic acids, each acid was positively indentified by the combined computer RI library search-AR comparison.

후 컬럼 동위원소 희석법을 적용한 HPLC-ICP/MS에서의 정량분석에서 내부 표준물을 이용한 정확도와 정밀도의 개선연구 (Study of improving precision and accuracy by using an internal standard in post column isotope dilution method for HPLC-ICP/MS)

  • 주민규;박명순;박용남
    • 분석과학
    • /
    • 제27권3호
    • /
    • pp.140-146
    • /
    • 2014
  • 후 컬럼 동위원소 희석법(PCID, post column isotope dilution)을 HPLC-ICP/MS (high performance liquid chromatography-inductively coupled plasma/mass spectrometry)에 적용한 정량법에서 내부 표준물을 동시에 사용하여 정확도와 정밀도를 개선하였다. 전통적인 여러 정량법과 후 컬럼 동위원소 희석법을 비교하여 볼 때에 PCID의 경우에 컬럼내에서 발생하는 오차가 가장 큰 요인으로 작용하였음을 알 수 있었다. PCID에서 내부 표준물을 사용하여 컬럼내에서의 손실에 대한 오차를 효과적으로 보정하고 정확도와 정밀도를 개선할 수 있었다. 셀레늄 화학종인 SeMet을 시료로 사용하고 내부 표준물로 MeSecys 또는 $Se^{4+}$를 이용한 결과, 사용하지 않은 경우와 비교하면 상대오차는 각 각 31%와 13%에서 모두 1% 대로 낮아져 정확도가 크게 개선되었으며, 상대 표준편차는 5.1%와 6.9%에서 각각 1.5%와 0.2%로 정밀도 또한 크게 개선되었다. PCID에서 내부 표준물을 사용하였을 때의 정량분석법의 장점을 다른 분석법과 비교 토의하였다.

Biplot of Ranked Data

  • Han, Sang-Tae;Huh, Myung-Hoe
    • Journal of the Korean Statistical Society
    • /
    • 제24권2호
    • /
    • pp.439-451
    • /
    • 1995
  • Ranked data are widely used in the area of social sciences, for instance in polls and preference surveys, in which a number of objects (or stimuli) are evaluted and ranked by a panel of judges (or subject) according to their preference. We propose a graphical method for ranked data by quantifying objects and judges. In a plot for judges, the interpoint distances can be interpreted as Spearman or Kendall distance between two rankings given by respective judges. Similarly, we also construct a plot for objects with a sensible relationship to the previous plot for judges.

  • PDF

Analytical Quality by Design Methodology Approach for Simultaneous Quantitation of Paeoniflorin and Decursin in Herbal Medicine by RP-HPLC Analysis

  • Kim, Min Kyoung;Park, Geonha;Hong, Seon-Pyo;Jang, Young Pyo
    • Natural Product Sciences
    • /
    • 제27권4호
    • /
    • pp.264-273
    • /
    • 2021
  • Simultaneous quantification of multiple marker compounds in herbal medicine by high performance liquid chromatography (HPLC) analysis is still a challenge due to the complexity in various parameters to be considered and co-existing multi-components. As a case study, a reliable HPLC method for simultaneous quantification of paeoniflorin from Paeoniae Radix and decursin from Angelicae Gigantis Radix in various commercial herbal medicine was developed based on analytical quality by design (AQbD) strategy. As a first step, risk assessment was performed to select the critical method parameters (CMPs) which were decided as organic mobile phase ratio and column oven temperature. In order to evaluate the effect of the CMPs on critical method attributes (CMAs) of peak resolution and tailing, central composite design (CCD) was employed. The final chromatographic conditions were optimized as follows: column- C18, 4.6 × 250 mm, 5 ㎛ particle size; mobile phase- A: acetonitrile, B: 0.1% acetic acid water; detection wavelength- 235 nm for paeoniflorin, 325 nm for decursin; column oven temperature- 25℃; flow rate- 1.0 mL/min; gradient mobile phase system as Time (min) : % A, 0:14, 25:14, 30:50, 60:50, 61:100, 65:100, 66:14, 75:14. The method was successfully validated according to the International Conference on Harmonization (ICH) guidelines and piloted for ten commercial herbal medicines.

A HPLC-UV method for quantification of ivermectin in solution from veterinary drug products

  • Kim, Young-Wook;Jeong, Wooseog
    • 한국동물위생학회지
    • /
    • 제45권3호
    • /
    • pp.243-248
    • /
    • 2022
  • The HPLC conditions for analysis of ivermectin in solutions dosage forms of commercial anthelmintics are different for each product. The purpose of this study was to establish a standardized chromatographic method for the quantification of ivermectin in solution. The separation was achieved on Waters Xbridge C18 column (4.6×150 nm, 5 ㎛) using different kinds of mobile phase composed of water/methanol/acetonitrile (15/34/51, v/v and 19.5/27.5/53, v/v), with UV detection at wavelengths 245 nm and 254 nm. A total of five commercial ivermectin in solution samples were analyzed. In this study, the optimal chromatographic conditions for analysis of ivermectin in solution were mobile phase of water/methanol/acetonitrile (15/34/51, v/v) at a flow rate of 1.0 mL/min and a detection wavelength of 245 nm using a Waters Xbridge C18 column (4.6×250 nm, 5 ㎛) at a column temperature of 25℃. The linearity was observed in the concentration range of 50~150 ㎍/mL, with a correlation coefficient, r2= 0.99999. The limit of detection and the limit of quantification were 0.88 and 2.68 ㎍/mL, respectively. The accuracy (% recovery) was found to be 98.9 to 100.3%. Intra-day and Intermediate precisions with relative standard deviations were less than 1.0%. The content of ivermectin for five market samples ranged 91.2~102.7%. The proposed method was also found to be robust, therefore, the method can be used for the routine analysis of ivermectin in solutions dosage forms.