• Title/Summary/Keyword: 감도 계수법

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Development and Validation of Analytical Method for Determination of Fungicide Spiroxamine Residue in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Spiroxamine의 시험법 개발 및 검증)

  • Park, Shin-Min;Do, Jung-Ah;Lim, Seung-Hee;Yoon, Ji-Hye;Pak, Won-Min;Shin, Hye-Sun;Kuk, Ju-Hee;Chung, Hyung-Wook
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.296-305
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    • 2018
  • Spiroxamine, one of fungicides, is used to control powdery mildew in various crops and black yellow sigatoka in bananas. The major strength of spiroxamine is to control powdery mildew in various crops and bananas yellow sigatoka in bananas. The compound has shown a high level of activity, good persistence and crop tolerance. Besides powdery mildew, good control of rust, net blotch and Rhynchosporium diseases been indicated in cereals, together with a complementary activity against Septoria diseases. In 2017, the maximum residue limit (MRL) of spiroxamine established in Korea. According to Ministry of ood and rug afety) regulations, spiroxamine residues defined only parent compound. Thus, a analytical method is needed to estimate the residue level of the parent compound. The objective of this study was to develop and validate analytical method for spiroxamine in representative agricultural commodities. Samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interfering substances. The analyte were quantified and confirmed liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive-ion mode using multiple reaction monitoring (MRM). Matrix matched calibration curves were linear over the calibration ranges ($0.0005{\sim}0.1{\mu}g/mL$) for the analyte in blank extract with coefficient of determination ($r^2$) > 0.99. For validation purposes, recovery studies will be carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries 70.6~104.6% with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges in the Codex guidelines (CAC/GL40, 2003) and MFDS guidelines. proposed analytical method be used as an official analytical method in the Republic of Korea.

A Case Study for the Estimation of Remaining Lives of Asphalt Pavements (아스팔트포장 잔존수명 예측 사례 연구)

  • Lee, Jung-Hun;Lee, Hyun-Jong;Park, Hee-Mun;Kim, In-Tai
    • International Journal of Highway Engineering
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    • v.10 no.2
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    • pp.1-13
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    • 2008
  • This study presents a case study of condition evaluation of various asphalt pavement sections to estimate performance lives. The pavement surface conditions including cracking and rutting are first evaluated using a automatic pavement analyzer, ARAN. HPCI(Highway Pavement Condition Index) values are estimated using the pavement surface distress data. It is observed from the pavement distress survey that the major distress type of the sections is top-down cracking. The modulus value of each pavement layer is back-calculated from the defection data obtained from a FWD(Falling Weight Deflectometer) and compared with the laboratory measured dynamic modulus values. Remaining lives of the various pavement sections are estimated based on a mechanistic-empirical approach and AAHTO 1993 design guide. The structural capacities of the all pavement sections based on the two approaches are strong enough to maintain the pavement sections for the rest of design life. Since the major distress type is top-down cracking, the remaining lives of the pavement sections are estimated based on HPCI and existing performance database of highway pavements. To evaluate the causes of premature pavement distress, various material properties, such as air void, asphalt binder content, aggregate gradation, dynamic modulus and fatigue resistance, are measured from the field cores. It is impossible to accurately estimate the binder contents of field samples using the ignition method. It is concluded from the laboratory tests that the premature top down cracking is mainly due to insufficient compaction and inadequate aggregate gradation.

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An Analysis of Sinking Resistance for Purse Seine - In the Case of the Model Seine with Different d/l - (선망의 침강 저항 해석 - d/l이 다른 모형망의 경우 -)

  • Kim, Suk-Jong;Park, Jeong-Sik
    • Journal of the Korean Society of Fisheries and Ocean Technology
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    • v.34 no.3
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    • pp.274-282
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    • 1998
  • This study deals with sinking resistance for purse seine, in the case of different d/l, ratio of twine diameter and leg length. Experiments carried out on the six types simplified reduced model seines which were made of knotless netting. The nettings were woven in different leg length 4.3, 5.0, 5.5, 6.0, 6.6 and 7.7mm of polyester 28 tex two threads two -ply twine, and each of the seines were named I, II, III, IV, V and Ⅵ seine. Dimension of seine models were 450cm for corkline and 85cm for seine depth, each seines rigged up 160g of float for a floatline and 50g (underwater weight) of lead for a leadline. Experiments were measured in the observation channel of a flume tank at the static conditions Sinking motion was recorded by the two sets TV-camera for VTR which were placed in top and side of the model seine, and reading coordinate carried out by the video digitization system. An analysis were calculated out by simultaneous differential equations for numerical method by Runge - Kutta - Gill sub - routine. The results obtained were as follows: 1. Average sinking speed of seine of seine margin was fastest for Ⅵ seine followed by V, IV, III, II and I seines. 2. The coefficient of resistance for a seine wall was depended upon the ratio of d/l : KD =0.081 (d/l )-0.5 3. The coefficient of resistance for netting bundle was not depended upon the ratio of d/l :CR = 0.91 (), d : Twine diameter, l : Leg length, : Density of netting materals, $\omega$ : Density of water

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Amperometric Determination of Anthracycline Antibiotics with the Mercury Film Thin Layer Flow Cell (수은피막 박막흐름전지를 이용한 Anthracycline계 항생제의 전류법 정량)

  • Kim, Kyung Eun;Hahn, Younghee
    • Analytical Science and Technology
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    • v.17 no.6
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    • pp.470-475
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    • 2004
  • The mercury film thin layer flow cell (MFTLFC) which yielded the highest sensitivity for the electrochemical reduction of doxorubicin was constructed by coating the glassy carbon working electrode (GCE; $A=0.208cm^2$) with $5{\mu}L$ of HgO coating solution (0.5% HgO + 0.25% polystyrene/cyclohexanone) and subsequently followed by applying a potential of -0.40 V for 300 sec in the flow stream of an acetate buffer of pH 4.5. The voltammogram of doxorubicin reached the diffusion current plateau at -0.53 V vs. a Ag/AgCl (3 M NaCl) in the MFTLFC. The diffusion current (Id) of doxorubicin at the MFTLFC was 1.7 times greater than the Id obtained at the TLFC employing a bare glassy carbon working electrode. When the peak areas (electric charge) were plotted vs. concentrations of standard anthracyclines, the calibration factors of doxorubicin and daunorubicin were $1.12{\times}10^8{\mu}C/M$ (coefficient of determination; $R^2$: 0.969) and $0.98{\times}10^8{\mu}C/M$> ($R^2$: 0.999), respectively in the concentration range between $1.0{\times}10^{-8}M$ and $1.0{\times}10^{-6}M$.

A Sensitive Detection of Actinide Species in Solutions Using a Capillary Cell (모세관 셀을 이용한 수용액 내 악티나이드 화학종의 고감도 검출)

  • Cho, Hye-Ryun;Park, Kyuong-Kyun;Jung, Euo-Chang;Song, Kyu-Seok
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.7 no.2
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    • pp.109-114
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    • 2009
  • Absorption spectra for a quantitative analysis of actinide elements such as U(VI) and Pu(V) were measured by using a liquid waveguide capillary cell (LWCC) which has an optical path length of 1.0 meter. In order to investigate radioactive elements, a LWCC is installed in a glove box and is coupled to a spectrophotometer with optical fibers. Limits of detection (LOD) for the system were determined as 0.74 and 0.35 M with molar absorption coefficients of 8.14${\pm}$0.07 (414 nm) and 17.00${\pm}$0.16 (569 nm) $M^{-1}cm^{-1}$ for U(VI) and Pu(V) ions, respectively. The measured LOD values are about 30 times more sensitive when compared to those achievable by using a conventional quartz cell with an optical path length of 1.0 cm. As an application with an enhanced sensitivity, a quantitative analysis for micromolar concentrations of Pu(V) has been performed to decrease the uncertainty in the formation constant of the Pu(VI)-OH complex.

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Improvement of an Analytical Method for Methoprene in Livestock Products using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 살충제 메토프렌의 잔류분석법 개선)

  • Park, Eun-Ji;Kim, Nam Young;Park, So-Ra;Lee, Jung Mi;Jung, Yong Hyun;Yoon, Hae Jung
    • Journal of Food Hygiene and Safety
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    • v.37 no.3
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    • pp.136-142
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    • 2022
  • The research aims to develop a rapid and easy analytical method for methoprene using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A simple, highly sensitive, and specific analytical method for the determination of methoprene in livestock products (beef, pork, chicken, milk, eggs, and fat) was developed. Methoprene was effectively extracted with 1% acetic acid in acetonitrile and acetone (1:1), followed by the addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. Subsequently, the lipids in the livestock sample were extracted by freezing them at -20℃. The extracts were cleaned using MgSO4, primary secondary amine (PSA), and octadecyl (C18), which were then centrifuged to separate the supernatant. Nitrogen gas was used to evaporate the supernatant, which was then dissolved in methanol. The matrix-matched calibration curves were constructed using 8 levels (1, 2.5, 5, 10, 25, 50, 100, 150 ng/mL) and the coefficient of determination (R2) was above 0.9964. Average recoveries spiked at three levels (0.01, 0.1, and 0.5 mg/kg), and ranged from 79.5-105.1%, with relative standard deviations (RSDs) smaller than 14.2%, as required by the Codex guideline (CODEX CAC/GL 40). This study could be useful for residue safety management in livestock products.

Development of a Simultaneous Analytical Method for Azocyclotin, Cyhexatin, and Fenbutatin Oxide Detection in Livestock Products using the LC-MS/MS (LC-MS/MS를 이용한 축산물 중 유기주석계 농약 Azocyclotin, Cyhexatin 및 Fenbutatin oxide의 동시시험법 개발)

  • Nam Young Kim;Eun-Ji Park;So-Ra Park;Jung Mi Lee;Yong Hyun Jung;Hae Jung Yoon
    • Journal of Food Hygiene and Safety
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    • v.38 no.5
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    • pp.361-372
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    • 2023
  • Organotin pesticide is used as an acaricide in agriculture and may contaminate livestock products. This study aims to develop a rapid and straightforward analytical method for detecting organotin pesticides, specifically azocyclotin, cyhexatin, and fenbutatin oxide, in various livestock products, including beef, pork, chicken, egg, and milk, using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The extraction process involved the use of 1% acetic acid in a mixture of acetonitrile and ethyl acetate (1:1). This was followed by the addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium chloride. The extracts were subsequently purified using octadecyl (C18) and primary secondary amine (PSA), after which the supernatant was evaporated. Organotin pesticide recovery ranged from 75.7 to 115.3%, with a coefficient of variation (CV) below 25.3%. The results meet the criteria range of the Codex guidelines (CODEX CAC/GL 40). The analytical method in this study will be invaluable for the analysis of organotin pesticides in livestock products.

Pyroelectric Properties of the $\beta$-PVDF (Poly(vilnylidene fluoride)) Thin Film Prepared by Vacuum Deposition with Applying Electric Field (전계인가 진공 증착법으로 제작된$\beta$ -PVDF (Poly(vinylidene fluoride)) 박막의 초전 특성)

  • Chang, Dong-Hoon;Kang, Seong-Jun;Yoon, Yung-Sup
    • Journal of the Institute of Electronics Engineers of Korea SD
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    • v.39 no.5
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    • pp.23-30
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    • 2002
  • The PVDF (Polyvinylidene Fluoride) thin film having P phase is prepared by the vacuum deposition with applying the electric field and its pyroelectric properties are studied by using a dynamic method to examine the possibility of the application to the pyroelectric IR sensor. The pyroelectric responses of the PVDF thin film are characterized as the frequency dispersion in both low and high modulation frequency regions, and their frequency dependences are observed. In the low frequency region (2~10Hzz), the polarization can easily rotate with the increase of modulation frequency and show the maximum since the reorientation rate of domains is higher than the modulation frequency. On the other hand, in the high frequency region (100~1000Hz), the pyroelectric response decreases as the frequency increases, because the reorienatation rate of domains is suppressed and thus, the change of polarization decreases. Pyroelectric coefficient, figure of merits for noise equivalent power and detectivity of the PVDF thin film are measured as 3.2$\times$10$^{-10}$ C/$\textrm{cm}^2$.K, 2.34$\times$10$^{-10}$ C.cm/J and 1.32$\times$10$^{-9}$ C.cm/J, respectively. Also, the noise equivalent and the detectivity are 1.66$\times$10$^{-7}$ W/H $z^{$\sfrac{1}{2}$}$, 6.03$\times$10$^{5}$ cm.H $z^{$\sfrac{1}{2}$}$W, respectively.

Simplification of One Step Immunotech AFP Test (AFP 검사방법 단축에 관한 고찰)

  • Moon, Ki Choon;Kwon, Won Hyun;Kim, Jung In;Lee, In Won
    • The Korean Journal of Nuclear Medicine Technology
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    • v.17 no.1
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    • pp.80-84
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    • 2013
  • Purpose: The Immunotech AFP is a widely used test in 14 hospitals(RIA QC establishments: 46) as a liver tumor marker. Normally, the test takes 45 minutes including complicated 2 step method. We evaluated the possibility of 1 step method and suitable test time. Materials and Methods: Samples of 31 patients in SNUBH were used as subject. We evaluated the sensitivity, intra and inter assay precision, recovery rate, linearity between 1 step and 2 step method (45 min. and 60 min.). Results: Both of 45 minutes and 60 minutes test showed 0.1 ng/mL sensitivity. In 45 minutes test, the intra assay coefficients of variation were 3.05%, 3.43%, 1.68%. Also, inter assay coefficients of variation were 3.91%, 2.38%, 0.82%. In 60 minutes test, the intra assay were 5.00%, 3.69%, 1.97%, inter assay were 3.14%, 3.71%, 1.85%.The correlation coefficient of each 2 step and 1 step (45 min.), 2 step and 1 step(60 min.), 1 step (45 min.) and 1 step (60 min.) were y=0.9293x+2.7356 ($R^{2}=0.9999$), y=0.9193x+4.1002 ($R^{2}=0.9993$), y=0.9894x+1.3805 ($R^{2}=0.9997$). Conclusion: Compared 1step method to 2 step method, both method showed very reasonable precision, recovery rate and correlation coefficient. Also, 1 step method(45 min.) of correlation coefficient ($R^2$) was 0.999. We suggest that 1 step method test can reduce the test time and is useful for AFP test.

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Determination of Amitrole in Water Samples by Evaporation and GC/MS (증발법과 GC/MS를 이용한 수질 시료 중의 Amitrole의 분석법 연구)

  • Yoon, So Hee;Hong, Ji Eun;Pyo, Hee Soo;Park, Song Ja
    • Analytical Science and Technology
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    • v.16 no.6
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    • pp.483-487
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    • 2003
  • Amitrole is well-known as a non-selective herbicide and it is able to cause contamination of driking water as well as pollution of ground water and surface water. However, it is difficult to extract from water because it has a high solubility for water whereas a low solubility for general organic solvents. This method is described for the determination of amitrole in water samples by GC/MS. After evaporation of 10 mL water sample by a vacuum evaporator, amitrole was derivatized with isobutyl chloroformate (iso-BCF) on room temperature for 15~20 min. As a result, the sensitivity for GCfMS was improved as N-isobutoxycarbonyl amitrole derivative was formed. The linearity of the calibration curve showed good as 0.997. The recoveries were obtained more than 94.9% and relative standard deviations were less than 2.8% at $1.0{\mu}g/L$, $10.0{\mu}g/L$ and $100.0{\mu}g/L$. The limit of detection showed $0.1{\mu}g/L$ with a signal-to-noise ratio (S/N) of 3.