• Title/Summary/Keyword: standard calibration

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Monitoring of Pesticides in the Yeongsan and Seomjin River Basin (영산강 및 섬진강 수계 중 농약 분포 조사)

  • Lee, Young-Jun;Choi, Jeong-Heui;Kim, Sang Don;Jung, Hee-Jung;Lee, Hyung-Jin;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.34 no.4
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    • pp.274-281
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    • 2015
  • BACKGROUND: A lasting release of low levels of persistence chemicals including pesticides and pharmaceuticals into river has a bad influence on aquatic ecosystems and humans. The present study monitored pesticide residues in the Yeongsan and Seomjin river basins and their tributaries as a fundamental study for water quality standard of pesticides.METHODS AND RESULTS: Nine pesticides(aldicarb, carbaryl, carbofuran, chlorpyrifos, 2,4-D, MCPA, methomyl, metolachlor, and molinate) were determined from water samples using SPE-Oasis HLB(pH 2) and LC/MS/MS. Validation of the method was conducted through matrix-matched internal calibration curve, method detection limit(MDL), limit of quantification(LOQ), accuracy, precision, and recovery. MDLs of all pesticides satisfied the GV/10 values. Linearity(r2) was 0.9965- 0.9999, and a percentage of accuracy, precision, and recovery was 89.4-113.6%, 3.1-14.0%, and 90.8-106.2%, respectively. All pesticides exclusive of aldicarb were determined in the river samples, and there was a connection between the positive monitoring results and agricultural use of the pesticides.CONCLUSION: Monitoring outcomes of the present study implied that pesticides were a possible non-point pollutant source in the Yeongsan and Seomjin river basins and tributaries. Therefore, it is required to produce and accumulate more monitoring results on pesticides in river waters to set water quality standards, finally to preserve aquatic ecosystems.

Determination of Carazolol and Azaperone in Livestock and Fishery Products Using Liquid Chromatography-tandem Mass Spectrometry (축수산물에서 LC-MS/MS를 이용한 카라졸롤 및 아자페론 분석)

  • Choi, Soo Yeon;Kang, Hui-Seung;Kim, Joohye;Cheon, So-Young;Jeong, Jiyoon;Cho, Byung-Hoon;Lee, Kang-Bong
    • Journal of Food Hygiene and Safety
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    • v.33 no.3
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    • pp.176-184
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    • 2018
  • The aim of the present work was to develop simultaneous methods of quantification of carazolol, azaperone, and azaperol residues in livestock and fishery products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Samples were extracted from beef, pork, chicken, egg, milk and shrimp using acetonitrile (ACN); while flat fish and eel were extracted using 80% ACN. For purification, ACN saturated n-hexane was used to remove fat composition. The standard calibration curves showed good linearity as correlation coefficients; $r^2$ was > 0.99. Average recoveries expressed were within the range of 67.9-105% for samples fortified at three different levels ($0.5{\times}MRL$, $1{\times}MRL$ and $2{\times}MRL$). The correlation coefficient expressed as precision was within the range of 0.55-7.93%. The limit of quantification (LOQ) was 0.0002-0.002 mg/kg. The proposed analytical method showed high accuracy and acceptable sensitivity based on Codex guideline requirements (CAC/GL71-2009). This method can be used to analyze the residue of carazolol, azaperone, and azaperol in livestock and fishery products.

Simultaneous Analysis Method of BPA, BPF, BADGE, BFDGE and Their Degradation Products in Canned Foods and Food Simulants by HPLC (HPLC를 이용한 캔 식품 및 식품 유사용매 중 BPA, BPF, BADGE, BFDGE 및 분해산물의 동시분석법)

  • Choi, Jae-Chun;Kyung, Suk-Hun;Lee, Gun-Tack;Lee, Kwang-Ho
    • Korean Journal of Food Science and Technology
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    • v.34 no.2
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    • pp.174-179
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    • 2002
  • A simple and sensitive analysis method based on reverse phase (RP) HPCL with flourescence detector was developed for simultaneous determination of bisphenol A (BPA), bisphenol F (BPF), bisphenol A diglycidyl ether (BADGE), bisphenol F diglycidyl ether (BFDGE), and their degradation products, $BADGE{\cdot}H_2O$, $BADGE{\cdot}2H_2O$, $BFDGE{\cdot}H_2O$, $BFDGE{\cdot}2H_2O$, $BADGE{\cdot}HCl{\cdot}H_2O$, $BADGE{\cdot}HCl$, $BADGE{\cdot}2HCl$, $BFDGE{\cdot}HCl{\cdot}H_2O$, $BFDGE{\cdot}HCl$ and $BFDGE{\cdot}2HCl$, which were hydrolyzed and chlorinated forms of BADGE and BFDGE, in canned foods and food simulants. These compounds were identified by GC/MSD with $MSTFA-NH_4I-DTE$ derivatization. Recovery study was performed at each 100 ng/mL levels of BPA, BPF, BADGE and BFDGE added to canned foods and food simulants. This method was resulted in recovery of $90{\sim}114%$ with relative standard deviation of $4.1{\sim}7.0%$, detection limits of $6{\sim}11$ ng/mL and quantitation limits of $12{\sim}18\;ng/mL$. Calibration curves were linear with correlatin coefficients of 0.997 for BPF, 0.996 for BPA, 0.9987 for BFDGE, and 0.9989 for BADGE.

Determination of Soluble Carbohydrates in Soybean Seeds Using High Performance Liquid Chromatography with Evaporative Light Scattering Detection (증기화광산란 검출기를 이용한 콩 함유 수용성 탄수화물의 분석)

  • Kim, Gyeong-Ha;Hwang, Young-Sun;Ahn, Kyung-Geun;Kim, Gi-Ppeum;Kim, Min-Ji;Hong, Seung-Beom;Moon, Jung-Kyeong;Choung, Myoung-Gun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.43 no.7
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    • pp.1062-1067
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    • 2014
  • In the present study, a new analytical method was devised for the simultaneous determination of soluble carbohydrates in soybean seeds using high performance liquid chromatography/evaporative light scattering detection (HPLC/ELSD). The limit of quantification (LOQ) for soybean soluble carbohydrates ranged from 5.6~7.6 mg/kg using the HPLC/ELSD method and from 16.2~33.9 mg/kg using the high performance liquid chromatography/refractive index detection (HPLC/RID) method. Therefore, the HPLC/ELSD method was more sensitive than HPLC/RID. The precision values for retention time and peak area of the HPLC/ELSD method were evaluated by inter-day (n=5) and intra-day (n=10) assays using a standard solution. All precision values (CV<2.5%) for soybean soluble carbohydrates were acceptable and fulfilled international acceptance criteria. All linear calibration curves were obtained with a correlation coefficient of $R^2$ >0.999. The contents of soluble carbohydrates for the "Shingikong" (yellow soybean) and "Cheongjakong 3" (black soybean) samples were analyzed using the HPLC/RID and HPLC/ELSD methods. The difference in carbohydrate contents between the two detection methods was significant. Carbohydrate contents in the HPLC/ELSD method were higher than those in the HPLC/RID method. Overall, the HPLC/ELSD method showed satisfactory resolution with a favorable LOQ and reproducibility. Therefore, these results indicate that the HPLC/ELSD method may be applied to determine the contents of soluble carbohydrates in soybean seeds and related food stuffs.

A Comparison Study of Aerosol Samplers for PM10 Mass Concentration Measurement (PM10 질량농도 측정을 위한 시료채취기의 비교 연구)

  • Park, Ju-Myon;Koo, Ja-Kon;Jeong, Tae-Young;Kwon, Dong-Myung;Yoo, Jong-Ik;Seo, Yong-Chil
    • Journal of Korean Society of Environmental Engineers
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    • v.31 no.2
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    • pp.153-160
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    • 2009
  • A PM10 (aerodynamic diameter${\leq}$10 ${\mu}m$) sampler is used to quantify the potential human exposure to suspended particulate matter (PM) and to comply with the governmental regulation. This study was conducted to compare and evaluate the same PM10 cutpoint and different slopes between United States Environmental Protection Agency (USEPA) PM10 sampling criterion and American Conference of Governmental Industrial Hygienists/$Comit\acute{e}$ $Europ\acute{e}en$ de Normalization/International Organization for Standardization thoracic PM10 sampling criterion through theory and experiment. Four PM10 samplers according to the USEPA criterion and one RespiCon sampler in accordance with the thoracic PM10 criterion were used in the present study. In addition, one DustTrak monitor was used to measure real time PM10 mass concentrations. All six aerosol samplers were tested in a PM generation chamber using polydisperse fly ash. Theoretical mass concentrations were calculated by applying the measured particle size distribution characteristics (geometric mean = 6.6 ${\mu}m$, geometric standard deviation = 1.9) of fly ash to each sampling criterion. The measured mass concentrations through a chamber experiment were consistent with theoretical mass concentrations in that a RespiCon sampler with the thoracic PM10 criterion collected less PM than a PM10 sampler with the USEPA criterion. The overall chamber experiment results indicated, when a PM10 sampler was used as a reference sampler, that (1) a RespiCon sampler had a normalizing factor of 1.6, meaning that this sampler underestimated an average 60% of PM10 mass sampled from a PM10 sampler, and (2) a DustTrak real-time monitor using a PM10 inlet had a calibration factor of 2.1.

Video Camera Characterization with White Balance (기준 백색 선택에 따른 비디오 카메라의 전달 특성)

  • 김은수;박종선;장수욱;한찬호;송규익
    • Journal of the Institute of Electronics Engineers of Korea SP
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    • v.41 no.2
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    • pp.23-34
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    • 2004
  • Video camera can be a useful tool to capture images for use in colorimeter. However the RGB signals generated by different video camera are not equal for the same scene. The video camera for use in colorimeter is characterized based on the CIE standard colorimetric observer. One method of deriving a colorimetric characterization matrix between camera RGB output signals and CIE XYZ tristimulus values is least squares polynomial modeling. However it needs tedious experiments to obtain camera transfer matrix under various white balance point for the same camera. In this paper, a new method to obtain camera transfer matrix under different white balance by using 3${\times}$3 camera transfer matrix under a certain white balance point is proposed. According to the proposed method camera transfer matrix under any other white balance could be obtained by using colorimetric coordinates of phosphor derived from 3${\times}$3 linear transfer matrix under the certain white balance point. In experimental results, it is demonstrated that proposed method allow 3${\times}$3 linear transfer matrix under any other white balance having a reasonable degree of accuracy compared with the transfer matrix obtained by experiments.

Development and Validation of Analytical Method for Determination of Biphenyl Analysis in Foods (식품 중 비페닐 분석법 개발 및 유효성 검증)

  • Kim, Jung-Bok;Kim, Myung-Chul;Song, Sung-Woan;Shin, Jae-Wook
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.4
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    • pp.459-464
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    • 2017
  • Biphenyl is used as an intermediate in the production of crop protection products, a solvent in pharmaceutical production, and as a component in the preservation of citrus fruits in many countries. Biphenyl is not authorized for use and also does not have standards or specifications as a food additive in Korea. National and imported food products are likely to contain biphenyl. Therefore, control and management of these products is required. In this study, a simple analytical method was developed and validated using HPLC to determine biphenyl in food. These methods are validated by assessing certain performance parameters: linearity, accuracy, precision, recovery, limit of detection (LOD), and limit of quantitation (LOQ). The calibration curve was obtained from 1.0 to $100.0{\mu}g/mL$ with satisfactory relative standard deviations (RSD) of 0.999 in the representative sample (orange). In the measurement of quality control (QC) samples, accuracy was in the range of 95.8~104.0% within normal values. The inter-day and inter-day precision values were less than 2.4% RSD in the measurement of QC samples. Recoveries of biphenyl from spiked orange samples ranged from 92.7 to 99.4% with RSD between 0.7 and 1.7% at levels of 10, 50, and $100{\mu}g/mL$. The LOD and LOQ were determined to be 0.04 and $0.13{\mu}g/mL$, respectively. These results show that the developed method is appropriate for biphenyl identification and can be used to examine the safety of citrus fruits and surface treatments containing biphenyl residues.

Determination of plasma C16-C24 globotriaosylceramide (Gb3) isoforms by tandem mass spectrometry for diagnosis of Fabry disease (패브리병(Fabry) 진단을 위한 혈장 중 Globotriaosylceramide (Gb3)의 탠덤매스 분석법 개발과 임상 응용)

  • Yoon, Hye-Ran;Cho, Kyung-Hee;Yoo, Han-Wook;Choi, Jin-Ho;Lee, Dong-Hwan;Zhang, Kate;Keutzer, Joan
    • Journal of Genetic Medicine
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    • v.4 no.1
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    • pp.45-52
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    • 2007
  • Purpose : A simple, rapid, and highly sensitive analytical method for Gb3 in plasma was developed without labor-ex tensive pre-treatment by electrospray ionization MS/ MS (ESI-MS/MS). Measurement of globotriaosy lceramide (Gb3, ceramide trihex oside) in plasma has clinical importance for monitoring after enzyme replacement therapy in Fabry disease patients. The disease is an X-linked lipid storage disorder that results from a deficiency of the enzyme ${\alpha}$-galactosidase A (${\alpha}$-Gal A). The lack of ${\alpha}$-Gal A causes an intracellular accumulation of glycosphingolipids, mainly Gb3. Methods : Only simple 50-fold dilution of plasma is necessary for the extraction and isolation of Gb3 in plasma. Gb3 in diluted plasma was dissolved in dioxane containing C17:0 Gb3 as an internal standard. After centrifugation it was directly injected and analyzed through guard column by in combination with multiple reaction monitoring mode of ESI-MS/MS. Results : Eight isoforms of Gb3 were completely resolved from plasma matrix. C16:0 Gb3 occupied 50% of total Gb3 as a major component in plasma. Linear relationship for Gb3 isoforms w as found in the range of 0.001-1.0 ${\mu}g$/mL. The limit of detection (S/N=3) was 0.001 ${\mu}g$/mL and limit of quantification was 0.01 ${\mu}g$/mL for C16:0 Gb3 with acceptable precision and accuracy. Correlation coefficient of calibration curves for 8 Gb3 isoforms ranged from 0.9678 to 0.9982. Conclusion : This quantitative method developed could be useful for rapid and sensitive 1st line Fabry disease screening, monitoring and/or diagnostic tool for Fabry disease.

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Analysis of Heavy Metals in $[^{201}Tl]$TICI Injection Using Polarography (폴라로그래피를 이용한 $[^{201}Tl]$염화탈륨 주사액의 중금속 분석)

  • Chun, Kwon-Soo;Suh, Yong-Sup;Yang, Seung-Dae;Ahn, Soon-Hyuk;Kim, Sang-Wook;Choi, Kang-Hyuk;Lee, Dong-Hoon;Lim, Sang-Moo;Yu, Kook-Hyun
    • The Korean Journal of Nuclear Medicine
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    • v.34 no.4
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    • pp.336-343
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    • 2000
  • Purpose: Thallous-201 chloride produced at Korea Cancer Center Hospital(KCCH) is used in detecting cardiovascular disease and cancer. Thallium impurity can cause emesis, catharsis and nausea, so the presence of thallium and other metal impurities should be determined. According to USP and KP, their amounts must be less than 2 ppm in thallium and 5 ppm in total. In this study, the detection method of trace amounts of metal impurities in $[^{201}Tl]$TICI injection with polarography was optimized without environmental contamination. Materials and Methods: For the detection of metal impurities, Osteryoung Square Wave Stripping Voltammetry method was used in Bio-Analytical System (BAS) 50W polarograph. The voltammetry was composed of Dropping Mercury Electrode (DME) as a working electrode, Ag/AgCl as a reference electrode and Pt wire as a counter electrode. Square wave stripping method, which makes use of formation and deformation of amalgam, was adopted to determine the metal impurities, and pH 7 phosphate buffer was used as supporting electrolyte. Results: Tl, Cu and Pb in thallous-201 chloride solution were detected by scanning from 300 mV to -800 mV Calibration curves were made by using $TINO_3,\;CuSO_4\;and\;Pb(NO_3){_2}$ as standard solutions. Tl was confirmed at -450 mV peak potential and Cu at -50 mV Less than 2 ppm of Tl and Cu was detected and Pb was not detected in KCCH-produced thallous-201 chloride injection. Conclusion: Detection limit of thallium and copper is approximately 50 ppb with this method. As a result of this experiment, thallium and other metal impurities in thallous-201 chloride injection, produced at Korea Cancer Center Hospital, are in the regulation of USP and KP Polarograph could be applied for the determination of metal impurities in the quality control of radiopharmaceuticals conveniently without environmental contamination.

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Mathematical Transformation Influencing Accuracy of Near Infrared Spectroscopy (NIRS) Calibrations for the Prediction of Chemical Composition and Fermentation Parameters in Corn Silage (수 처리 방법이 근적외선분광법을 이용한 옥수수 사일리지의 화학적 조성분 및 발효품질의 예측 정확성에 미치는 영향)

  • Park, Hyung-Soo;Kim, Ji-Hye;Choi, Ki-Choon;Kim, Hyeon-Seop
    • Journal of The Korean Society of Grassland and Forage Science
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    • v.36 no.1
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    • pp.50-57
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    • 2016
  • This study was conducted to determine the effect of mathematical transformation on near infrared spectroscopy (NIRS) calibrations for the prediction of chemical composition and fermentation parameters in corn silage. Corn silage samples (n=407) were collected from cattle farms and feed companies in Korea between 2014 and 2015. Samples of silage were scanned at 1 nm intervals over the wavelength range of 680~2,500 nm. The optical data were recorded as log 1/Reflectance (log 1/R) and scanned in intact fresh condition. The spectral data were regressed against a range of chemical parameters using partial least squares (PLS) multivariate analysis in conjunction with several spectral math treatments to reduce the effect of extraneous noise. The optimum calibrations were selected based on the highest coefficients of determination in cross validation ($R^2{_{cv}}$) and the lowest standard error of cross validation (SECV). Results of this study revealed that the NIRS method could be used to predict chemical constituents accurately (correlation coefficient of cross validation, $R^2{_{cv}}$, ranging from 0.77 to 0.91). The best mathematical treatment for moisture and crude protein (CP) was first-order derivatives (1, 16, 16, and 1, 4, 4), whereas the best mathematical treatment for neutral detergent fiber (NDF) and acid detergent fiber (ADF) was 2, 16, 16. The calibration models for fermentation parameters had lower predictive accuracy than chemical constituents. However, pH and lactic acids were predicted with considerable accuracy ($R^2{_{cv}}$ 0.74 to 0.77). The best mathematical treatment for them was 1, 8, 8 and 2, 16, 16, respectively. Results of this experiment demonstrate that it is possible to use NIRS method to predict the chemical composition and fermentation quality of fresh corn silages as a routine analysis method for feeding value evaluation to give advice to farmers.