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Simultaneous analysis of glucocorticoids in bovine muscle and liver by LC-MS/MS (LC-MS/MS를 이용한 소의 근육과 간 중에 잔류하는 glucocorticoids 동시 분석)

  • Shin, Sang-Eun;Cho, Hyun-Woo;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.23 no.4
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    • pp.405-413
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    • 2010
  • A new method for the simultaneous determination of six glucocorticoids (betamethasone, dexamethasone, prednisone, prednisolone, methylprednisolone, and flumethasone) in meats (bovine muscle, bovine liver) were established. Samples were effectively extracted using C18 cartridge with ethylacetate. Chromatographic separation was achieved using C18 column and negative electrospray ionization mass spectrometry was performed in the Multiple Reaction Monitoring mode for the effective quantitation and qualification of glucocorticoids. Acetonitrile and water (0.1% formic acid) were used as mobile phase and additive for effective electrospray ionization, and gave good chromatographic separation and mass spectrometric sensitivity. The limit of detection (LODs) and the limit of quantitation (LOQs) in spiked blank samples depending on types of matrix and pharmaceuticals were ranged from 0.2 to $1.0\;{\mu}g$/kg and 0.8 to $3.4\;{\mu}g$/kg, respectively. And the recoveries were between 89.5 to 119.6%. The established method showed good recoveries, accuracies, precisions and fast sample preparation and it will be applied to assay of glucocorticoids residues in meat.

Improvement of Power Consumption of Canny Edge Detection Using Reduction in Number of Calculations at Square Root (제곱근 연산 횟수 감소를 이용한 Canny Edge 검출에서의 전력 소모개선)

  • Hong, Seokhee;Lee, Juseong;An, Ho-Myoung;Koo, Jihun;Kim, Byuncheul
    • The Journal of Korea Institute of Information, Electronics, and Communication Technology
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    • v.13 no.6
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    • pp.568-574
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    • 2020
  • In this paper, we propose a method to reduce the square root computation having high computation complexity in Canny edge detection algorithm using image processing. The proposed method is to reduce the number of operation calculating gradient magnitude using pixel's continuity using make a specific pattern instead of square root computation in gradient magnitude calculating operation. Using various test images and changing number of hole pixels, we can check for calculate match rate about 97% for one hole, and 94%, 90%, 88% when the number of hole is increased and measure decreasing computation time about 0.2ms for one hole, and 0.398ms, 0.6ms, 0.8ms when the number of hole is increased. Through this method, we expect to implement low power embedded vision system through high accuracy and a reduced operation number using two-hole pixels.

Quantitative analysis of 3-MCPD in water using LC-MS (LC-MS를 이용한 수용액중의 3-MCPD 정량)

  • Park, Gyo-Beom;Kim, Yong-Hwa;Kim, Jin-Sung;Jeong, Ja-Young;Kim, Choong-Yong;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.198-203
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    • 2007
  • The analysis method of 3-Monochloropropane-1,2-diol (3-MCPD) compound in water was developed using liquid chromatography with mass spectrometric detection. Aqueous solution was controlled in strong basic condition with sodium hydroxide, and then $25{\mu}L$ of benzoyl chloride was added to the solution for the derivatization of 3-MCPD. The derivative was extracted using pentane and analyzed by the selected ion monitoring (SIM) method of LC-MS. The results of analyses showed that the calibration curves was in the range of 1.0 to $100{\mu}g/mL$ with a good linearity (correlation coefficient of $r^2=0.992$) and limit of detection was below $0.01{\mu}g/mL$. The recoveries of this analysis method by LC-MS were 92.3-98.0 %.

Analysis of Heterocyclic Amines in Mainstream Cigarette Smoke using by LC-MS/MS (LC-MS/MS를 이용한 담배 연기 중 Heterocyclic Amines의 분석)

  • Kim, Ick-Joong;Jang, Gi-Chul;Ji, Sang-Un;Min, Hye-Jeong;Kim, Hyo-Keun;Hwang, Geon-Jung
    • Journal of the Korean Society of Tobacco Science
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    • v.30 no.1
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    • pp.33-38
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    • 2008
  • This study was carried out to determine the analytical methods for heterocyclic amines(HAs) of the tobacco smoke by LC/MS/MS. HAs have been found in pyrolysate of protein and cooked food including protein, were known the Sugimura compound. HAs content of the smoke were known to exist very low ppb level. Especially, some of HAs are mutagenic and carcinogenic compounds. In according to IARC, the toxicity of N-heterocyclic amines classified IARC class 2A or 2B group. Precursors of these compounds are glutamic acid, protein and free amino acids including tryptophan, therefore, the precursors have been proved in cooked food continuously. This study was investigate multiple analysis methods for HAs and HAs contents of some commercial products. In this study, we used the linear type smoking machine for HAs analysis. At the ISO conditions, mainstream smoke was collected on cambridge filter pad, and then cambridge filter pad was extracted by 0.1% acetic acid. The extracted solution were passed cation exchange SPE cartridge to remove matrix, samples were analyzed using LC/MS/MS on MRM mode. From the result that optimized this methods, the correlation coefficient(R) of the individual compounds were good linearity over 0.999, recovery rate over 96% and the limit of detection were good values between 0.06 to 0.37 ng/mL, In addition, HAs content of some commercial products were in range of 0.02 to 43.8 ng/cig.

Simultaneous Determination of 80 Unapproved Compounds using HPLC and LC-MS/MS in Dietary Supplements

  • Kwon, Jeongeun;Shin, Dasom;Kang, Hui-Seung;Suh, Junghyuck;Lee, Gunyoung;Lee, Eunju
    • Mass Spectrometry Letters
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    • v.13 no.3
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    • pp.58-83
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    • 2022
  • We developed analytical methods using high performance chromatography (HPLC) and liquid chromatography tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of 80 unapproved compounds in dietary supplements. The target compounds for analysis were unapproved ingredients (e.g., pharmaceuticals) that have potential adverse effects on consumers owing to accidental misuse, overuse, and interaction with other medication in dietary supplement. Two analytical methods were tested to identify the optimal validation results according to AOAC guideline. As a result, limit of quantification (LOQ) was 0.14-0.5 ㎍ mL-1; linearity (r2) was ≥ 0.99; accuracy (expressed as recovery) was 78.9-114%; precision (relative standard deviation) was ≤ 4.28% in the HPLC method. In the LC-MS/MS method, LOQ was 0.01-2 ng mL-1, linearity (r2) was ≥0.98, accuracy was 71.7-119%; precision was ≤ 12.5%. The developed methods were applied to 51 dietary supplements collected from 2019 to 2021 through MFDS alert system. Based on our previous monitoring study, major compounds were icariin, sibutramine, yohimbine, sildenafil, tadalafil, sennosides (A, B), cascarosides (A, B, C, D), and phenolphthalein. In this study, we re-analyzed samples of detected compounds, and evaluated the statistical difference using Bland-Altman analysis to compare two analytical approaches between HPLC and LC-MS/MS. These results showed a good agreement between two methods that can be used to monitor the unapproved ingredients in dietary supplements. The developed two methods are complementarily suitable for monitoring the adulteration of 80 unapproved compounds in dietary supplements.

Quantification of the 25 Components in Onkyung-Tang by Ultra Performance Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry (UPLC-ESI-MS/MS를 이용한 온경탕 중 25종 성분의 함량분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.47 no.1
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    • pp.92-101
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    • 2016
  • In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was established for simultaneous determination of the 25 marker components, including chlorogenic acid, gallic acid, oxypaeoniflorin, homogentisic acid, methyl gallate, caffeic acid, 3,4-dihydroxybenzaldehyde, paeoniflorin, albiflorin, liquiritin, nodakenin, ferulic acid, ginsenoside Rg1, liquiritigenin, coumarin, cinnamic acid, benzoylpaeoniflorin, ginsenoside Rb1, cinnamaldehyde, paeonol, glycyrrhizin, 6-gingerol, evodiamine, rutecarpine, and spicatoside A in traditional Korean formula, Onkyung-tang. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was carried out using a Waters ACQUITY TQD LC-MS/MS coupled with an electrospray ionization (ESI) source in the positive and negative modes. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$, respectively. The correlation coefficient of all analytes in the test ranges was greater than 0.98. The limits of detection and quantification values of the 25 marker compounds were in the ranges 0.03-19.43 and 0.09-58.29 ng/mL, respectively. As a result, methyl gallate, 3,4-dihydroxybenzaldehyde, evodiamine, and rutecarpine were not detected in this sample and the concentrations of the 21 compounds except for the above 4 compounds were $33.09-3,496.32{\mu}g/g$ in Onkyung-tang decoction. Among these compounds, paeonol was detected at the highest amount as a $3,496.32{\mu}g/g$.

A Study on the Fabrication Process and Magnetic Properties of Buble Magnetic Materials. (버블자성재료의 제조 및 자기 특성에 관한 연구)

  • Park, Yong-Du;Kim, Jong-O
    • Korean Journal of Materials Research
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    • v.5 no.8
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    • pp.1040-1044
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    • 1995
  • Magnetic garnet films of (YSmLuCa)$_3$(FeGe)$\_$5/O$\_$12/ have been grown by the liquid phase eqitaxy method on the substrate of non-magnetic garnet Gd$_3$Ga$\_$5/O$\_$12/. The variation of Sm ion concentration were varied 0.3, 0.4, 0.6, mole/formula unit respectively. The magnetic properties of the samples for the bubble magnetic materials, such as, line width ΔH of ferromagnetic resonance (FMR), magnetic saturation induction 4$\pi$Ms, wall mobility u$\_$w/ uniaxial magnetic anisotropy energy Ku, were measured and discussed the relations between these properties. The line width ΔH decreases with increasing 4$\pi$Ms, and with decreasing Sm concentration. The anisotropy energy Ku increases not only with increasing Sm ion concentration, but also increasing 4$\pi$Ms. The value of wall mobility u$\_$w/ increase with increasing 4$\pi$Ms and decreases with increasing Sm concentration. We define a physical constant Eι from the fact that the product of 4$\pi$Ms and ΔH is constant with dimension of energy density. The Eι is dependent only on Sm concentration.density. The Eι is dependent only on Sm concentration.

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Agreement between Smartphone Addiction and Perceived Smartphone Addiction among Adolescents (청소년의 스마트폰 중독수준과 중독인식간의 일치도)

  • Kim, Sohyun;Jeong, Ihn Sook
    • The Journal of Korean Society for School & Community Health Education
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    • v.15 no.2
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    • pp.91-101
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    • 2014
  • Objectives: This study aimed to identify agreement between smartphone addiction (SA) and perceived SA among adolescents. Methods: This survey was done with 394 subjects conveniently sampled from elementary school (ES), middle school (MS), academic (AHS) and vocational (VHS) high school. The data were collected from June 20 to July 20, 2013 with self-administered questionnaire and analyzed by descriptive statistics, chi-square test and Cohen's kappa (${\kappa}$). Results: High risk of SA showed 2.8% in total, 1.0% in ES, 2.1% in MS, 4.1% in AHS, and 4.0% in VHS, which was statistically different by type of school (p<0.001). Perceived SA showed 22.6% in total, 9.0% in ES, 21.9% in MS, 33.7% in AHS, and 26.0% in VHS, which was statistically different by type of school (p=0.003). The agreement between SA and perceived SA was 82.0% (${\kappa}$=0.54) in total, 91.8% (${\kappa}$=0.53) in ES, 75.0% (${\kappa}$=0.33) in MS, 77.5% (${\kappa}$=0.53) in AHS, and 84.8% (${\kappa}$=0.65) in VHS. Conclusion: The agreement between SA and perceived SA showed moderate in general, but fair in MS. It is suggested to develop step-by-step activities to reduce the gap between SA and perceived SA among adolescen, in particular, middle school students.

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Evaluation of Electrocardiographic Index in Healthy Raccoon Dogs (Nyctereutes procyonoides) (건강한 너구리(Nyctereutes procyonoides)들의 심전계 지표에 대한 평가)

  • Hong, Won-Woo;Kim, Jong-Taek;Yang, Dong-Keun;Nam, Hyo-Seung;Hyun, Changbaig
    • Journal of Veterinary Clinics
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    • v.30 no.6
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    • pp.456-458
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    • 2013
  • The aim of this study is to evaluate the reference value for electrocardiogram in healthy captive raccoon dogs. Forty-one free-ranging adult raccoon dogs rescued from Wildlife rescue centre, Kangwon National University were enrolled in this study. The 6-lead electrocardiogram was obtained in all raccoon dogs without any chemical restraints. The mean heart rate was $146.10{\pm}43.31$ beats/min (95% confidence interval 132.84~159.36 beats/min). The mean respiration rate was $35.73{\pm}11.56$ breaths/min (95% confidence interval 32.19~39.27 breaths/min). The mean systolic blood pressure was $136{\pm}29.26$ mmHg (95% confidence interval 127.99~145.91 mmHg). Electrocardiographical features were also evaluated in all raccoon dogs. The mean duration and amplitude of P-wave were $38.2{\pm}4.0$ ms (range 28-40 ms) and $0.128{\pm}0.039$ mV (range 0.09~0.20). The mean duration and amplitude of QRS complexes were $48.5{\pm}7.2ms$ (range 36-60 ms) and $1.330{\pm}0.650$ mV (range 0.15~2.30). The range of the mean electrical (QRS) axis was $-91^{\circ}{\sim}+96^{\circ}$ ($10^{\circ}{\sim}60^{\circ}$; 95% of confidence interval). The mean corrected QT (QTc) interval was $273.7{\pm}32.7ms$ (range 212-333 ms), while the mean PR interval was $76.1{\pm}10.0ms$ (range 50-82 ms). To the authors' knowledge, this is the first study to provide references in electrocardiogram (ECG) in healthy captive raccoon dogs.

Development and validation of an analytical method for pyrimisulfan determination in agricultural commodities by LC-MS/MS (LC-MS/MS를 이용한 농산물 중 pyrimisulfan 잔류량 분석법 개발 및 확인)

  • Do, Jung-Ah;Lee, Mi-Young;Cho, Yoon-Jae;Kang, Iil-Hyun;Kwon, Kisung;Oh, Jae-Ho
    • Analytical Science and Technology
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    • v.26 no.2
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    • pp.154-163
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    • 2013
  • The maximum residue limits of pyrimisulfan is set as 0.05 mg/kg in rice in 2011, so very reliable and sensitive analytical method for pyrimisulfan residues is required for ensuring the food safety of pyrimisulfan residues in agricultural products. In this study, a rapid and sensitive analytical method was developed and validated using liquid chromatography electrospray ionization tandem mass spectrometry (LC-MS/MS) for the determination of herbicide pyrimisulfan residues in agricultural products. Average recoveries of pyrimisulfan ranged from 88.7 to 99.3% at the spiked level of 0.005 mg/kg and from 90.1 to 94.2% at the spiked level of 0.05 mg/kg, while the relative standard deviation was less than 10%. Linear range of pyrimisulfan was between 0.01~1.0 ${\mu}g/mL$ with the correlation coefficient ($r^2$) 0.999 and limit of quantification was 0.005 mg/kg. The results of method validation were satisfied Codex guideline. The results revealed that the developed and validated analytical method is possible for pyrimisulfan determination in agricultural product samples and will be used as an official analytical method.