• Title/Summary/Keyword: phase detection

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Determination of Free 4-hydroxyproline with Dansylchloride by HPLC in Human Urine (소변 중 4-hydroxyproline 분석에 관한 연구)

  • Lee, Keou-Weon;Cho, Young-Bong;Lee, Kyung-Jong
    • Journal of Preventive Medicine and Public Health
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    • v.35 no.4
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    • pp.282-286
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    • 2002
  • Objectives : The level of 4-hydroxyproline (4-Hyp) in human urine was measured using high performance liquid chromatography (HPLC) with a fluorescence detector. This method is useful for medical examinations and investigating the radicals induced by physical, chemical, mental stresses. This method is superior to many published several methods in terms of its low cost and ability to analyze many samples. Methods : The urine from workers in a tire manufacturing company (22 male pre- and post-shift workers) and 18 office-workers as controls were analyzed. Data concerning age, the cumulative drinking amount and the cumulative smoking amount was collected with a questionnaire. The optimum applied amount of dansyl-Cl, the optimum reaction temperature and time, the recoveries and the optimum pH of the eluent and buffer were determined.4-Hyp from human urine was derivatized with dansyl-Cl (dimethylamino-naphthalene-1-sulfonyl chloride) after removing the a-amino acid by a treatment with phthalic dicarboxaldehyde (OPA) and cleaned with Bond Elut C18 column. The 4-Hyp derivatives were separated on a reversed phase column by gradient elution with a phosphate buffer (5 mmol, pH 8.0) and acetonitrile, and detected by fluorescence measurements at 340 nm (excitation) and 538 nm (emission). Results : The detection limit for the urinary free 4-Hyp was $0.364{\mu}mol/l$. The recovery rate of 4-Hyp was 99.7%, and the effective pH of the phosphate buffer and borate buffer were 3.0 and 8.0, respectively. From statistical analysis, age, drinking and smoking did not affect the urinary free 4-Hyp in both the controls and workers. The range of urinary 4-Hyp in the controls, pre-shift, and post-shift workers were 0.33-16.44, N.D-49.06, and $0.32-56.27{\mu}mol/l$. From the pared-sample t-test, the urinary 4-Hyp levels in post-shift workers ($11.82{\pm}6.73\;nmmol/mg\;Cre$) were 2-fold higher than in pre-shift workers ($5.36{\pm}5.53\;nmol;/mg\;Cre$) and controls ($4.91{\pm}4.89\;nmol;/mg\;Cre$). Conclusions : This method was developed with high sensitivity, accuracy, and precision. The present method was effectively applied to analyze the urinary free 4-Hyp in both controls and workers.

Study on Signal Processing in Eddy Current Testing for Defects in Spline Gear (스플라인 기어부 결함의 와전류검사 신호처리에 관한 연구)

  • Lee, Jae Ho;Park, Tae Sung;Park, Ik Keun
    • Journal of the Korean Society for Nondestructive Testing
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    • v.36 no.3
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    • pp.195-201
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    • 2016
  • Eddy current testing (ECT) is commonly applied for the inspection of automated production lines of metallic products, because it has a high inspection speed and a reasonable price. When ECT is applied for the inspection of a metallic object having an uneven target surface, such as the spline gear of a spline shaft, it is difficult to distinguish between the original signal obtained from the sensor and the signal generated by a defect because of the relatively large surface signals having similar frequency distributions. To facilitate the detection of defect signals from the spline gear, implementation of high-order filters is essential, so that the fault signals can be distinguished from the surrounding noise signals, and simultaneously, the pass-band of the filter can be adjusted according to the status of each production line and the object to be inspected. We will examine the infinite impulse filters (IIR filters) available for implementing an advanced filter for ECT, and attempt to detect the flaw signals through optimization of system design parameters for detecting the signals at the system level.

Simultaneous Determination of Synephrine and N-Methyltyramine in Orange Fruit and Juice from Korean Market by UPLC-FLD (UPLC-FLD를 이용한 국내 시판 오렌지 및 오렌지 주스 중 시네프린 및 n-메틸티라민 동시분석)

  • Kim, Hyo Jin;Kwak, Byung-Man;Ahn, Jang-Hyuk;Park, Jong-Su
    • Korean Journal of Food Science and Technology
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    • v.46 no.3
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    • pp.276-282
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    • 2014
  • An accurate and sensitive analytical method was established for the simultaneous determination of synephrine and n-methyltyramine contents by ultra-performance liquid chromatography (UPLC) with a fluorescence detector (FLD). A 70:30 (v/v) mixture of 10 mM sodium dodecyl sulfate (SDS) and acetonitrile was used as the mobile phase. The coefficient of correlation ($r^2$) was 0.9999 for both synephrine and n-methyltyramine, and their limits of detection (LOD) were 0.02 and 0.01 mg/kg, respectively. The percentage recoveries for synephrine and n-methyltyramine were 96.4% and 100.9%, respectively, from bitter orange (Citrus aurantium) samples. The synephrine and n-methyltyramine contents were 38.07-118.21 mg/kg and 0.27-0.56 mg/kg, respectively, in the orange fruit samples, while they were 14.61-120.39 mg/kg and up to 3.34 mg/kg, respectively, in the tested commercial orange juice samples. The differences in synephrine and n-methyltyramine content between orange fruit and commercial orange juice were not significant (p<0.05). These results suggest that UPLC-FLD can be applied to develop an analytical method of quality control for commercial orange juice.

Development of an Official Method for Measurement of Fluazinam Residues for Quarantine of Imported and Exported Horticultural Products (수출입 원예작물의 검역을 위한 살균제 Fluazinam의 공정 잔류분석법 개발)

  • Kim, Gyeong-Ha;Ahn, Kyung-Geun;Kim, Gi-Ppeum;Hwang, Young-Sun;Chang, Moon-Ik;Kang, In-Kyu;Lee, Young Deuk;Choung, Myoung-Gun
    • Horticultural Science & Technology
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    • v.34 no.1
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    • pp.183-194
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    • 2016
  • This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was $0.004mg{\cdot}kg^{-1}$ in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.

Development and Validation of Analytical Methods for Picoxystrobin Determination in Agricultural Products by GC-ECD and GC-MS

  • Do, Jung-Ah;Lee, Min-Hye;Park, Hyejin;Kang, Il-Hyun;Kwon, Kisung;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.27 no.4
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    • pp.332-338
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    • 2012
  • A simple and sensitive analytical method was developed using gas chromatography with electron capture detector (GC-ECD) and gas chromatography-mass spectrometry (GC-MS) for determination of Picoxystrobin in agricultural products (apple, hulled rice, mushroom, pepper, soybean, and mandarin). Picoxystrobin residues were extracted with acetonitrile, partitioned with saline water, and then they were cleaned up on a florisil solid-phase extraction (SPE) cartridge to obtain an extract suitable for analysis by GC-ECD and GC-MS. The method was validated using 6 agricultural product samples spiked with Picoxystrobin at different concentration levels (0.02, 0.05 and 0.5 mg/L). Average recoveries of Picoxystrobin (using each concentration three replicates) ranged 64.0~98.3% with relative standard deviations less than 10%, calibration solutions concentration in the range 0.1~5 mg/L, and limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.02 mg/L, respectively. The result showed that the developed analytical method is suitable for Picoxystrobin determination in agricultural products.

Development of the Analytical Method for Diazepam in Fishery Products using Liquid and Gas Chromatography-tandem Mass Spectrometry (LC-MS/MS 및 GC-MS/MS를 활용한 수산물 중 디아제팜의 정량분석법 개발)

  • Shin, Dasom;Kang, Hui-Seung;Kim, Joohye;Jeong, Jiyoon;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.33 no.2
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    • pp.110-117
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    • 2018
  • The aim of this study was to develop an analytical method for the quantification of diazepam residues in fishery products, using liquid and gas chromatography-tandem mass spectrometry (LC-MS/MS and GC-MS/MS). The sample utilized in the study was extracted from the fish sample (crucian carp) using 0.1% formic acid in acetonitrile. For the utilization of the purification process, the dispersive solid phase extraction (dSPE) was used for LC-MS/MS, dSPE and SPE was used for GC-MS/MS, respectively. To be sure, the standard calibration curves showed a good linearity as the noted correlation coefficients, $r^2$ was > 0.99. The average recoveries for accuracy ranged in 99.8~124% for the samples which were fortified at three different levels (0.001, 0.002 and 0.010 mg/kg). The correlation coefficient for the precision effect was measured at a range of 4.01~11.8%. The limit of detection (LOD) for the diazepam analysis was 0.0004 mg/kg, and the limit of the quantification (LOQ) was 0.001 mg/kg. The proposed analytical method was characterized with a high accuracy and acceptable sensitivity to meet the established Codex Alimentarius Commission (CAC/GL71-2009) guideline requirements. We therefore established the optimal analysis method for the determination of diazepam in the fishery products using LC-MS/MS and GC-MS/MS. It would be applicable to analyze the diazepam residues in fishery products in further studies on this subject.

Determination of Carbendazim in Commercial Agricultural Products by LC-MS/MS (LC-MS/MS를 이용한 농산물 중 카벤다짐 분석)

  • Hwang, Lae-Hwong;Lee, Sung-Deuk;Kim, Jeong-Gon;Kim, Ji-Young;Park, So-Hyun;Kim, Ji-Hae;Park, Jung-Hyun;Han, Chang-Ho;Kim, Mu-Sang
    • Journal of Food Hygiene and Safety
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    • v.32 no.2
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    • pp.141-146
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    • 2017
  • A rapid and precise method using LC-MS/MS was developed for carbendazim analysis in agricultural products. This compound was extracted with acetonitrile from agricultural products and cleaned up by solid-phase extraction procedure. The limit of detection and quantification were 0.001 mg/kg and 0.004 mg/kg, respectively. The mean recoveries and precision from 4 agricultural products, soybean sprout and mungbean sprout were in the range of 83.3-86.4% and 0.2-3.0% spiked at 1.0 mg/kg and those were in the range of 77.3-90.1% and 1.3-3.8% spiked at 0.02 mg/kg. The present method is faster and more precise compared with the multi-residue method of Korean Food Code. Therefore, we conclude that this method is suitable for carbendazim determination in a wide range of agricultural products.

Studies on the Determination Method of Hydrogen Peroxide in Foods (식품 중 과산화수소의 분석법에 관한 연구)

  • Lee, Tal-Soo;Lee, Young-Ja;Park, Jae-Seok;Kwon, Yong-Kwan;Hwang, Jung-Yeon;Lee, Ju-Yeun;Lee, Chul-Won
    • Korean Journal of Food Science and Technology
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    • v.34 no.6
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    • pp.998-1001
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    • 2002
  • Micro-LC method for the quantitative determination of hydrogen peroxide in foods has been established. This method was carried out on cation-exchange resin gel column using distilled water as mobile phase with 50 mM sodium sulfate as electrolyte. The detection was performed with an electrochemical detector (ECD) at 0.6 voltage. Under this analytical condition, the recovery rates of hydrogen peroxide in tomato and lemon were 98.3 and 97.4%, respectively. Among 28 food types, hydrogen peroxide concentrations were 0.6, 0.5, 1.9, 0.9, 0.5, 0.6, 0.9, 0.8, and 0.4 ppm in banana, peach, orange, strawberry, pepper, onion, cucumber, burdock, and egg plant, respectively, Whereas none was detected in remaing 19 samples.

Diagnosis and Prognosis of Sepsis (패혈증의 진단 및 예후예측)

  • Park, Chang-Eun
    • Korean Journal of Clinical Laboratory Science
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    • v.53 no.4
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    • pp.309-316
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    • 2021
  • Sepsis is a physiological response to a source of infection that triggers mechanisms that compromise organ function, leading to death if not treated early. Biomarkers with high sensitivity, specificity, speed, and accuracy that could differentiate sepsis from non-infectious systemic inflammatory response syndrome (SIRS) could bring about a revolution in sepsis treatment. Given the limitations and time required for microbial verification of pathogens, the accurate diagnosis of infection before employing antibiotic therapy is important and clinically necessary. Procalcitonin (PCT), lactate, C-reactive protein (CRP), cytokines, and proadrenomedullin (ProADM) are the common biomarkers used for diagnosis. The procalcitonin (PCT)-guided antibiotic treatment in patients with acute respiratory infections effectively reduces antibiotic exposure and side effects while improving survival rates. The evidence regarding sepsis screening in hospitalized patients is limited. Clinicians, researchers, and healthcare decision-makers should consider these findings and limitations when implementing screening tools, future research, or policy on sepsis recognition in hospitalized patients. The use of biomarkers in pediatric sepsis is promising, although such use should always be correlated with clinical evaluation. Biomarkers may also improve the prediction of mortality, especially in the early phase of sepsis, when the levels of certain pro-inflammatory cytokines and proteins are elevated.

Change in Physical Properties depending on Contaminants and Introduction to Case Studies of Geophysical Surveys Applied to Contaminant Detection (오염원에 따른 오염지역 물성 변화 및 물리탐사 적용 사례 소개)

  • Yu, Huieun;Kim, Bitnarae;Song, Seo Young;Cho, Sung Oh;Caesary, Desy;Nam, Myung Jin
    • Geophysics and Geophysical Exploration
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    • v.22 no.3
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    • pp.132-148
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    • 2019
  • Recently, safety and environmental concerns have become major social issues. Especially, a special underground-safety law has been made and enacted to prevent ground subsidence around construction sites. For environmental problems, several researches have started or will start on characterization of contaminated sites, in-situ environmental remediation in subsurface, and monitoring of remediation results. As a part of the researches, geophysical surveys, which have been mainly applied to explore mineral resources, geological features or ground, are used to characterize not only contaminated areas but also fluid flow paths in subsurface environments. As a basic study for the application of geophysical surveys to detect contamination in subsurface, this paper analyzes previous researches to understand changes in geophysical properties of contaminated zones by various contaminants such as leachate, heavy metals, and non-adequate phase liquid (NAPL). Furthermore, this paper briefly introduces how geophysical surveys like direct-current electrical resistivity, induced polarization and ground penetration radar surveys can be applied to detect each contamination, before analyzing case studies of the applications in contaminated areas by NAPL, leachate, heavy metal or nitrogen oxides.