• 제목/요약/키워드: Linearity assessment

검색결과 79건 처리시간 0.025초

Determination of Heterocyclic Amines and Acrylamide in Agricultural Products with Liquid Chromatography-Tandem Mass Spectrometry

  • Lee, Kyung-Jun;Lee, Gae-Ho;Kim, HaeSol;Oh, Min-Seok;Chu, Seok;Hwang, In Ju;Lee, Jee-yeon;Choi, Ari;Kim, Cho-il;Park, Hyun-Mee
    • Toxicological Research
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    • 제31권3호
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    • pp.255-264
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    • 2015
  • Heterocyclic amines (HCAs) and acrylamide are unintended hazardous substances generated by heating or processing of foods and are known as carcinogenic and mutagenic agents by the animal experiments. A simple method was established for a rapid and accurate determination of 12 types of HCAs (IQ, MeIQ, Glu-P-1, Glu-P-2, MeIQx, Trp-P-1, Trp-P-2, PhIP, $A{\alpha}C$, $MeA{\alpha}C$, Harman and Norharman) and acrylamide in three food matrices (non-fat liquid, non-fat solid and fat solid) by isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS). In every sample, a mixture of internal standards including $IQ-d_3$, $MeIQx-d_3$, $PhIP-d_3$, $Trp-P-2-^{13}C_2-^{15}N$ and $MeA{\alpha}C-d_3$ was spiked for quantification of HCAs and $^{13}C_3$-acrylamide was also spiked for the analysis of acrylamide. HCAs and acrylamide in sample were extracted with acetonitrile and water, respectively, and then two solid-phase extraction cartridges, ChemElut: HLB for HCAs and Accucat: HLB for acrylamide, were used for efficiently removing interferences such as pigment, lipid, polar, nonpolar and ionic compounds. Established method was validated in terms of recovery, accuracy, precision, limit of detection, limit of quantitation, and linearity. This method showed good precision (RSD < 20%), accuracy (71.8~119.1%) and recovery (66.0~118.9%). The detection limits were < 3.1 ng/g for all analytes. The correlation coefficients for all the HCAs and acrylamide were > 0.995, showing excellent linearity. These methods for the detection of HCAs and acrylamide by LC-MS/MS were applied to real samples and were successfully used for quantitative monitoring in the total diet study and this can be applied to risk assessment in various food matrices.

원전 증기발생기 와전류검사 장치의 전기적 특성 측정 (Electrical Characteristics Measurement of Eddy Current Testing Instrument for Steam Generator in NPP)

  • 이희종;조찬희;유현주;문균영;이태훈
    • 비파괴검사학회지
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    • 제33권5호
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    • pp.465-471
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    • 2013
  • 원전 증기발생기는 원자로 냉각재 계통에서 발생한 열에너지를 터빈 계통의 주급수에 전달하여 터빈을 회전시키기 위한 증기를 생산하는 일종의 열교환기이다. 증기발생기 전열관의 손상은 증기발생기의 구조적 및 누설 건전성 유지 능력을 저해시키기 때문에 주기적으로 와전류검사를 수행하여 전열관의 건전성을 평가한다. 증기발생기 전열관의 건전성 평가는 보통 원자로 연료 재장전 기간 중에 수행된다. 현재 국내 증기발생기 전열관에 적용되는 와전류검사는 KEPIC 및 ASME 코드 요건에 따라 수행되며, 와전류검사 수행에 필요한 검사 시스템은 와전류검사 장치와 수집된 신호를 평가하기 위한 평가 프로그램으로 구성된다. 검사에 적용되는 와전류검사 시스템을 구성하는 핵심기기인 와전류검사 장치는 ASME 및 KEPIC 코드에서 총 고조파 왜곡율, 입출력 임피던스, 증폭기 직선성 및 안정성, 위상 직선성, 대역폭 및 복조필터 응답, 디지털 변환, 채널 간섭 등과 같은 전기적 특성을 측정하도록 규정하고 있다. 이에 따라 본 논문에서는 국내 최초로 개발한 원전 증기발생기 와전류검사 장치의 전기적 특성 측정을 위한 ASME 및 KEPIC 코드 요건을 설명하고, 이 요건에 따른 증기발생기 와전류검사 장치의 전기적 특성의 측정 결과를 제시하였다.

Dog 혈장 중 HPLC-ICP/MS를 이용한 비소 화학종 분석법 검증 (Bioanalytical method validation for determination of arsenic speciation in dog plasma using HPLC-ICP/MS)

  • 김종환;권영상;신민철;김수정;서종수
    • 분석과학
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    • 제29권5호
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    • pp.234-241
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    • 2016
  • 비글견 혈장 중 arsenite (As(III)), arsenate (As(V)), dimethylarsinic acid (DMA)와 monomethylarsonic acid (MMA)를 정량하기 위한 분석법의 유효성을 검증하기 위하여 본 연구를 수행하였다. 비소를 종 분리하기 위하여 액체크로마토그래피 (HPLC) 와 결합된 유도결합 플라즈마 질량분석기 (ICP/MS) 를 사용하였으며, 비소를 정량하는 검출기에서 스펙트럼 간섭을 최소화하기 위하여 산소(O2)를 반응기체로 하는 DRC (dynamic reaction cell)모드를 이용하였다. 분석법의 유효성을 검증하는 항목으로 선택성, 직선성, 정확성, 정밀성, 생체시료효과, 회수율, 시스템 적합성, 희석의 타당성과 안정성 실험을 실시하였다. 선택성의 결과 정량에 방해되는 피크는 없는 것으로 확인 되었으며, 정량범위에서 평균 상관계수가 0.999 이상의 좋은 직선성을 보였다. 최저정량한계는 As(III), As(V)와 DMA는 5 ng/mL이였고, MMA는 20 ng/mL이였다. 생체시료의 영향, 시스템 적합성 과 회수율 항목을 통해 정량성에 대한 영향이 없음을 확인하여 비글견 혈장 중 비소 종을 분리하여 정량하는 분석법의 유효성을 검증하였다. 따라서 본 연구에서 제시한 분석법은 건강에 유해한 비소의 농도를 정량 및 평가하는데 적용될 것이다.

개선된 응답면기법에 의한 신뢰성 평가 (Reliability Assessment Based on an Improved Response Surface Method)

  • 조태준;김이현;조효남
    • 한국강구조학회 논문집
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    • 제20권1호
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    • pp.21-31
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    • 2008
  • 응답면기법(RSM, Response surface method)은 복잡한 구조물의 매우 작은 발생확률이나 신뢰성해 석에서 폭넓게 사용된다. MCS(Monte-Carlo Simulation)방법은 어떤 시스템의 평가에서도 사용될 수 있으나 해석시간이 파괴확률의 역수에 비례하게 되어 발생확률이 매우 희박한 시스템의 평가에 불리하다. 확률유한요소해석법은 이러한 MCS의 한계점을 해결해 줄 수 있는 대안이 될 수 있다. 그러나 이 방법은 평균과 표준편차 등이 모델링 (내부 프로그래밍)된 특별한 프로그램에서만 적용 가능하며 임의의 범용소프트웨어의 응답을 모델링하거나 임의의 프로그램의 특성을 이용할 수가 없다. RSM방법은 복잡한 구조시스템에서 응답에 대한 회귀모델을 구성하여 효율적인 해석단계를 통해 시간과 노력을 획기적으로 절감시킬 수 있다. 그러나 RSM의 정확도는 한계상태방정식의 선형성과 축점간의 거리에 영향을 받게 된다. 이런 단점을 해결하기 위해 한계상태방정식의 선형성과 무관하게 정확한 수렴해를 구하기 위한 개선된 적응적 응답면기법을 개발하고 선형과 2차형식의 응답면방정식에 대한 2가지 예를 들어 검증하였다. 검증결과 가장 효율적인 RSM기법을 결정하였다. 개발된 선형적응적가중응답 면기법 (linear adaptive weighted response surface method, LAW-RSM)은 비적응적이거나 비가중형식의 2차 RSM기법에 비해서 정해의 신뢰성지수에 가장 근접한 정확성과 수렴성을 나타낸다.

소아 치과진정법 시행 시 진정심도 감시를 위한 Cerebral State Monitor의 임상적 유용성 (Clinical Usefulness of Cerebral State Monitor for Monitoring Sedation Depth during Dental Sedation in Children)

  • 신터전;현홍근;김영재;김정욱;장기택;이상훈;김종철;서광석
    • 대한치과마취과학회지
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    • 제14권1호
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    • pp.11-15
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    • 2014
  • Background: It is imperative that adequate sedation level should be maintained for safe and effective dental sedation. Cerebral state index (CSI) is a empirically derived parameter calculated from the processed electroencephalography (EEG). We investigated whether CSI can be used as a sedation depth indicator. Methods: We continuously recorded CSI and bispectral index (BIS) values from 10 healthy children aged 3.6 yr undergoing dental sedation. We also evaluated sedation level using the Modified Observer's Assessment of Alertness/Sedation (MOAA/S). The correlation between CSI and BIS, or CSI and sedation score were sought a regression analysis. Results: There were good linearity between CSI values and sedation score. (r = 0.916, P < 0.001) The paired CSI and BIS values showed a significant correlation between the two values. (r = 0.895, P < 0.001) The difference between CSI and BIS values was not statistically significant at deep and conscious sedative levels. Conclusions: The CSI monitor can be easy to monitor sedation depth during dental sedation for children.

Activity and Safety Recognition using Smart Work Shoes for Construction Worksite

  • Wang, Changwon;Kim, Young;Lee, Seung Hyun;Sung, Nak-Jun;Min, Se Dong;Choi, Min-Hyung
    • KSII Transactions on Internet and Information Systems (TIIS)
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    • 제14권2호
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    • pp.654-670
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    • 2020
  • Workers at construction sites are easily exposed to many dangers and accidents involving falls, tripping, and missteps on stairs. However, researches on construction site monitoring system to prevent work-related injuries are still insufficient. The purpose of this study was to develop a wearable textile pressure insole sensor and examine its effectiveness in managing the real-time safety of construction workers. The sensor was designed based on the principles of parallel capacitance measurement using conductive textile and the monitoring system was developed by C# language. Three separate experiments were carried out for performance evaluation of the proposed sensor: (1) varying the distance between two capacitance plates to examine changes in capacitance charges, (2) repeatedly applying 1 N of pressure for 5,000 times to evaluate consistency, and (3) gradually increasing force by 1 N (from 1 N to 46 N) to test the linearity of the sensor value. Five subjects participated in our pilot test, which examined whether ascending and descending the stairs can be distinguished by our sensor and by weka assessment tool using k-NN algorithm. The 10-fold cross-validation method was used for analysis and the results of accuracy in identifying stair ascending and descending were 87.2% and 90.9%, respectively. By applying our sensor, the type of activity, weight-shifting patterns for balance control, and plantar pressure distribution for postural changes of the construction workers can be detected. The results of this study can be the basis for future sensor-based monitoring device development studies and fall prediction researches for construction workers.

랫트뇨중의 Alanine Aminopeptidase와 $\beta$-Glucuronidase 측정에 의한 신장독성 평가에 관하여 (Nephrotoxicity Assessment by Determination of Alanine Aminopeptidase (AAP) and $\beta$-Glucuronidase(GRS) in Rat)

  • 신동환;이창우
    • 한국임상수의학회지
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    • 제8권1호
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    • pp.31-45
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    • 1991
  • Present experiment was performed in order to establish the optimal reaction conditions for determination of urinary AAP and GRS activities and to investigate the applicability of urinary AAP and GRS in nephrotoxicity test in rat. The results were as follows ; 1. The optimal pH of phosphate buffer for determination of urinary AAP activity was 7.8. 2. The Michaelis constant of urinary AAP ranged from 0.8 to 1.0mmol/$\ell$ 3. The optimal wave length for determination of urinary GRS activity was 405nm. 4. The optimal pH of acetate buffer for determination of urinary GRS activity was 5.6. 5. The Michaelis constant of urinary GRS ranged from 0.65~0.79mmo1/$\ell$. 6. The AAP activities in gel-filtered samples were significantly higher than those in crude samples. Mean values of AAP activities in gel-filtered samples and crude samples were 29$\pm$20 and 20$\pm$13U/$\ell$, respectively. 7. There was not significant difference between gel-filtered samples and crude samples in urinary GRS activities. Mean values of GRS activities in gel-filtered samples and crude samples were 57$\pm$40 and 56$\pm$39U/$\ell$, respectively. 8. Limits of linearity of urinary AAP and GRS activities were 2.0 and 3.6U/$\ell$, respectively. 9. Within-run imprecisions of the assays, were acceptable, as the coefficients of the AAP activities ranged from 5.5 to 6.3% and those of GRS activities ranged from 1.4 to 6.2%, respectively. 10. Urinary AAP excretion was 675$\pm$227mu/24hrs.kg before administration of potassium dichromate, and increased significantly to 4246$\pm$2567mU/24hrs.kg within 24 hours after administration of potassium dichromate. 11. Urinary GRS excretion did not increase significantly after administration of potassim dichromate. 12. From these findings it is concluded that urinary AAP excretion is early and sensitive Indicator to detect kidney damage in nephrotoxicity experiment.

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도시지역 사무실내 공기 중 환경담배연기의 측정 - 흡연이 부유먼지 농도에 미치는 영향을 중심으로 - (Measurement of Environmental Tobacco Smoke in the Air of Offices in Urban Areas - Focusing on the Impact of Smoking on the Concentrations of Suspended Particles -)

  • 백성옥;박상곤
    • 한국대기환경학회지
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    • 제20권6호
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    • pp.715-727
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    • 2004
  • This study was carried out to evaluate non-smoker's exposure levels to environmental tobacco smoke (ETS) in the air of offices in urban areas. A total of 65 offices were selected from two large cities, i.e. Daegu and Daejeon. The field sampling was conducted repeatedly in summer (1999) and winter (1999~2000). The measured ETS markers included respirable suspended particles (RSP as PM$_{40}$ ), vapor and particulate phase ETS markers, including nicotine, 3-ethnyl pyridine (3-EP), ultraviolet absorbing particulate matter (UVPM), fluorescing particulate matter (FPM), and solanseol in ETS particles (SolPM). RSP was measured gravimetrically by a microbalance. The particle samples were then used for the determination of particulate ETS markers by HPLC, while vapor phase markers determined by GC/NPD. The analytical methods were validated for repeatability, linearity, detection limits, and duplication precision. The concentrations of RSP and other ETS markers were significantly higher in smoking offices than non-smoking offices. Despite the similar smoking strength in each office for different seasons, the concentration levels of ETS components appeared to be higher in winter than summer. The contributions of ETS to RSP concentrations based on SolPM, FPM, and UVPM methods were estimated to be in the range of 15.2 ~ 25.3% in smoking offices, whereas 2.4 ~ 15.9% in non-smoking offices. The cooling and heating types did not affect significantly the concentrations of RSP and other ETS markers. Finally, further research issues were suggested to obtain more scientific information on the non-smoker's exposure to ETS with respect to the frame of risk assessment..

LC-ESI-MS/MS를 이용한 계지탕 중 주요 성분 분석 (Quantitative Determination of the Bioactive Marker Components in Gyeji-tang Using LC-ESI-MS/MS)

  • 서창섭;하혜경
    • 생약학회지
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    • 제49권1호
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    • pp.76-83
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    • 2018
  • A traditional herbal formula, Gyeji-tang has been used to treat the early colds, headache, chills, and fever in Asian countries. In this study, we were performed simultaneous determination of the 14 bioactive marker compounds, gallic acid, spinosin, paeoniflorin, albiflorin, liquiritin apioside, liquiritin, 6'''-feruloylspinosin, liquilitigenin, coumarin, cinnmamic acid, benzoylpaeoniflorin, cinnamaldehyde, glycyrrhizin, and 6-gingerol in Gyeji-tang using an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS). Analytical column was used a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) and maintained at $45^{\circ}C$ with a flow rate of 0.3 mL/min. The mobile phase consists of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was conducted using multiple reaction monitoring in the positive and negative modes by a Waters ACQUITY TQD LC-MS/MS system. The calibration curves of 14 bioactive marker compounds showed linearity with correlation coefficients ${\geq}0.9798$. The limits of detection and quantification values were in the range of 0.11-6.66 ng/mL and 0.34-19.99 ng/mL, respectively. As a result of the analysis using the established LC-MS/MS method, the amounts of tested 14 compounds in the lyophilized Gyeji-tang sample were detected up to $85.7{\mu}g/g$. These results may be useful for quality assessment of a traditional herbal formulas.

Rapid characterization of ginsenosides in the roots and rhizomes of Panax ginseng by UPLC-DAD-QTOF-MS/MS and simultaneous determination of 19 ginsenosides by HPLC-ESI-MS

  • Wang, Hong-Ping;Zhang, You-Bo;Yang, Xiu-Wei;Zhao, Da-Qing;Wang, Ying-Ping
    • Journal of Ginseng Research
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    • 제40권4호
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    • pp.382-394
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    • 2016
  • Background: Ginsenosides are the characteristic and principal components which manifest a variety of the biological and pharmacological activities of the roots and rhizomes of Panax ginseng (GRR). This study was carried out to qualitatively and quantitatively determine the ginsenosides in the cultivated and forest GRR. Methods: A rapid and sensitive ultra-high-performance liquid chromatography coupled with diode-array detector and quadrupole/time of flight tandem mass spectrometry (UPLC-DAD-QTOF-MS/MS) was applied to the qualitative analysis of ginsenosides and a 4000 QTRAP triple quadrupole tandem mass spectrometer (HPLC-ESI-MS) was applied to quantitative analysis of 19 ginsenosides. Results: In the qualitative analysis, all ingredients were separated in 10 min. A total of 131 ginsenosides were detected in cultivated and forest GRR. The method for the quantitative determination was validated for linearity, precision, and limits of detection and quantification. 19 representative ginsenosides were quantitated. The total content of all 19 ginsenosides in the forest GRR were much higher than those in the cultivated GRR, and were increased with the growing ages. Conclusion: This newly developed analysis method could be applied to the quality assessment of GRR as well as the distinction between cultivated and forest GRR.