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Verification of Analytical Method of Azaspiracid Toxins in Shellfish and Tunicates by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS (Liquid Chromatography-Tandem Mass Spectrometry)를 이용한 패류 및 피낭류 중 아자스필산 분석법의 유효성 검증)

  • Cho, Sung Rae;Jeong, Sang Hyeon;Park, Kunbawui;Yoon, Minchul;Kim, Dong Wook;Son, Kwang Tae;Ha, Kwang Soo
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.54 no.4
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    • pp.404-410
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    • 2021
  • Although, mouse bioassay for the monitoring of azaspiracids (AZAs) toxins in shellfish has been used previously, the reported method has low sensitivity and it is time-consuming. Recently, there is an interest in the quantitative analysis of AZAs using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The purpose of this study is to verify the simultaneous analysis of AZAs in shellfish and tunicate in Korea using LC-MS/MS. To validate the method, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and repeatability were determined. All standard compounds were analyzed within 7 min. The correlation coefficients (R2) of the standard solution was higher than 0.9995 (within the range of 0.8-10.0 ㎍/L). The LODs and LOQs of AZAs in shellfish were 0.08-0.16 ㎍/kg and 0.23-0.50 ㎍/kg, respectively. The accuracy and precision of the method for determining AZAs in shellfish were 87.1-93.0% and 1.23-4.91%, respectively. Consequently, the verified LC-MS/MS method is suitable to analyze AZAs in shellfish and tunicates in Korea.

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

  • Seo, Chang-Seob;Ha, Hyekyung
    • Korean Journal of Pharmacognosy
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    • v.49 no.1
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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.

Simultaneous determination of parabens in cosmetics by LC/MS (LC/MS를 이용한 화장품 중의 parabens 동시 분석 방법 연구)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.23 no.1
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    • pp.54-59
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    • 2010
  • The simultaneous analysis of parabens in cosmetic samples was carried out by LC/MS. The cosmetic samples are directly dissolved in methanol and filterated using $0.45\;{\mu}m$ filter. The methanol-water was used for the mobile phase of gradient conditions. An Extend $C_{18}$ reverse-phase column and the selected ion monitoring (SIM) mode were applied. The analysis results of LC/MS showed good linearity with correlation coefficient of $r^2$=0.9993 in the range of 0.05 to $10\;{\mu}g$/mL and detection limit of $0.01\;{\mu}g$/mL.

Sex Determination Using a Discriminant Analysis of Maxillary Sinuses and Three-Dimensional Technology

  • Jeong-Hyun Lee;Hee-Jeung Jee;Eun-Seo Park;Seok-Ho Kim;Sung-Suk Bae
    • Journal of dental hygiene science
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    • v.22 no.4
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    • pp.249-255
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    • 2022
  • Background: Sexual dimorphism is important for sex determination in the field of forensics. However, sexual dimorphism is commonly assessed using cone beam computed tomography (CBCT) rather than three-dimensional (3D) modeling software; therefore, studies using a more accurate measurement approach are necessary. This study assessed the sexual dimorphism of the MS using a 3D modeling program to obtain information that could contribute to the fields of surgery and forensics. Methods: The CBCT data of 60 patients (age, 20~29 y; 30 males and 30 females) admitted to the Department of Orthodontics at the Dankook University School of Dentistry were provided in Digital Imaging and Communications in Medicine (DICOM) format. The left MS and right MS were modeled based on the DICOM files using the Mimics (version 22; Materialise, Leuven, Belgium) 3D program and converted to stereolithography (STL) files used to measure the width, length, and height of the MS, infraorbital foramen (IOF), right MS, and left MS. The average of three repeated measurements was calculated, and a reliability test was performed to ensure data reliability (Cronbach's α=0.618). A canonical discriminant analysis was performed using a standard approach (left: Box's M=0.096; right: Box's M=0.115). Results: Males had greater values for all parameters (MS width, MS length, MS height, IOF, right MS, left MS) than females. The discriminant analysis identified six independent variables (MS width, MS height, MS length, IOF, right MS, left MS) that could identify sex. The left MS and right MS correctly identified the sex of 81.7% and 71.7% of the patients, respectively, with the left MS having higher accuracy. Conclusion: This study confirmed that, for Korean individuals, the left MS has a better ability to identify sex than the right MS. These results may contribute to sex identification in the fields of surgery and forensics.

Determination of Trace-Level Perchlorate by IC-MS/MS and Distribution in the Han River (IC-MS/MS를 이용한 수중의 과염소산이온 분석방법 최적화 및 한강수계내 분포조사)

  • Kim, Hyun-Hee;Han, Ihn-Sup;Jeong, Gwan-Jo;Park, Hyeon;Han, Sun-Hee;Cho, Wan-Seon
    • Journal of Korean Society of Environmental Engineers
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    • v.32 no.4
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    • pp.349-356
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    • 2010
  • Ion chromatography (IC) coupled with conductivity detector (CD) is a common system for the determination of perchlorate in water samples. Although the IC method with CD has been widely used for the determination of trace level perchlorate ion in water, sensitivity decreases dramatically as the complexity of the matrices increases. Here we proposed the application of ion chromatography coupled with mass spectrometry (IC-MS/MS) to significantly improve selectivity of perchlorate. The mean recovery of the method was 104.4 ${\pm}$ 5.7% and the relative standard deviation (RSD%) was 1.9 ${\pm}$ 1.3%. The alculated method detection limit (MDL) was 0.0207 ${\pm}$ 0.0099 ${\mu}g/L$. The concentrations of perchlorate were minimum <0.1 ${\mu}g/L$ and maximum 18.3 ${\mu}g/L$ in source water (Namhan, Bukhan and Han River). Hongreung showed higher concentrations ($1^{st}$-14.3 ${\mu}g/L$, $2^{st}$-18.3 ${\mu}g/L$) than the other places. And the concentrations of perchlorate were 0.18~0.34 ${\mu}g/L$ in the samples taken from the six water treatment plants and six intake stations in Seoul.

Micropropagation of Heloniopsis orientalis (Thunb.) C. Tanska in vitro (조직배양을 이용한 처녀치마[Heloniopsis orientalis (Thunb) C. Tanaka] 대량 증식)

  • 윤세영;이명선;임상철;신중두
    • Korean Journal of Plant Tissue Culture
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    • v.27 no.3
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    • pp.197-202
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    • 2000
  • The effect of cultural media and growth regulators on multiple plant regeneration from leaf explants of Heloniopsis orientalis (Thunb.) Tanaka was evaluated. The highest percentage of shoot and root formation were 20 and 30% on MS medium treated at 3.0 mg $l^{-1}$ of zeatin, respectively. Also 67 and 33% of high shoot formation appeared on 1/2 MS and 5 culture medium treated at zeatin 1.0 and 3.0 mg $l^{-1}$ respectively. With MS treated at 0.5 mg $l^{-1}$ of 2,4-D 1/2 MS and B5 culture media treated at each 1.0 and 3.0 mg $l^{-1}$ of zeatin the highest ratios of plant produced were 100, 280 and 310 % respectively relative to the other treatments. Generally, there was highest possibility for multiple propagation of Heloniopsis orientalis (Thunb.) C. Tanaka with B5 culture media supplemented 3.0 mg $l^{-1}$ of zeatin.

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Evaluation of the Method for Total Homocysteine in Plasma Using LC-MS/MS (LC-MS/MS를 이용한 Homocysteine 측정과 그 유용성 평가)

  • Jun, Sun-Hee;Lim, Mi-Suk;Jung, Yong-Sun;Song, Jung-Han
    • Korean Journal of Clinical Laboratory Science
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    • v.37 no.1
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    • pp.22-26
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    • 2005
  • Total homocysteine is now considered a risk factor for cardiovascular diseases. I increased interest has led to a multitude of studies requiring the determination of total homocysteine in conjunction with other factor. There are various methods for measuring total homocysteine, including HPLC, FPIA, GC-MS and LC-MS/MS. The most recent method for measuring total homocysteine uses a deuterium-labelled internal standard and tandem mass spectrometry. This development requires no derivatization and therefore leads to an increase in sample throughput compared to other techniques. We have evaluated the method for homocysteine by the LC-MS/MS method, and the correlation between the FPIA method and the LC-MS/MS method. The standard curve (0, 5, 10, 20, 50, 100 uM) was linear over the range examined (up to 100 uM). The lower limit of quantification (CV < 10 %) was 0.5 uM/L and the lower limit of detection (S/N >3) was 0.1 uM/L. Intra-assay variation and inter-assay variation were both <6 %. The comparision study for homocysteine concentration showed good correlation (r=0.9684) between the FPIA method and LC-MS/MS methods. Our conclusion is that the method showed relatively good precision, and was rapid and accurate.

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Effects of Expanding Feed Processing Technologies on Egg Characteristic and Nutrient Digestibility in Laying Hens (Expanding 사료 가공 기술이 산란계의 계란 품질 및 영양소 소화율에 미치는 효과)

  • Yoo J.S.;Chae S.J.;Park S.E.;Jang H.D.;Seok H.B.;Kim I.H.;Kim Y.C.
    • Korean Journal of Poultry Science
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    • v.33 no.2
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    • pp.127-131
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    • 2006
  • This study was conducted to investigate the effects of expanding feed processing technologies on the egg characteristics and nutrient digestibility in laying hens. A total of two hundred seventy laying hens were randomly allocated into three treatments with fifteen replications for six weeks. Dietary treatments include 1) MS(mash), 2) EC(expanded crumble) and 3) EP(expanded pellet). In the egg production, the EC and EP treatments were significantly higher than MS treatment(p<0.05). However, no significant difference was founded in egg weight(p>0.05). Egg shell breaking was increased in EC and EP treatments compared with MS treatment(p<0.05), however, egg shall thickness showed no significant difference(p>0.05). Egg production and egg shell breaking were significantly higher in EC and EP treatments than MS treatment(p<0.05), but egg weight and egg shell thickness were no significantly difference among treatment(p<0.05). Yolk color was increased in EC treatment compared with other treatments(p<0.05). Also, yolk index was significantly improved in EC and EP treatments compared with MS treatment(p<0.05). Haugh unit was increased in EC treatment compared with MS treatment(p<0.05). EC treatment had improved DM, Ca and P digestibility. In conclusion, Expanded crumble and pellet processing could improve the egg characteristic and nutrient digestibility in laying hens.

Quantitative Analysis of Brain Metabolite Spectrum Depending on the Concentration of the Contrast Media in Phantom (팬텀 내 조영제 농도에 따른 뇌 대사물질 Spectrum의 정량분석)

  • Shin, WoonJae;Gang, EunBo;Chun, SongI
    • Journal of the Korean Society of Radiology
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    • v.9 no.1
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    • pp.47-53
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    • 2015
  • Quantitative analysis of MR spectrum depending on mole concentration of the contrast media in cereberal metabolite phantom was performed. PRESS pulse sequence was used to obtain MR spectrum at 3.0T MRI system (Archieva, Philips Healthcare, Best, Netherland), and the phantom contains brain metabolites such as N-Acetyl Asparatate (NAA), Choline (Cho), Creatine (Cr) and Lactate (Lac). In this study, optimization of MRS PRESS pulse sequency depending on the concentration of contrast media (0, 0.1 and $0.3mmol/{\ell}$) was evaluated for various repetition time(TR; 1500, 1700 and 2000 ms). In control (cotrast-media-free) group, NAA and Cho signals were the highest at TR 2000 ms than at 1700 and 1500 ms. Cr had the highest peak signal at TR 1500 ms. When concentration of contrast media was $0.1mmol/{\ell}$, the metabolites were increased NAA 73%, Cho 249%, Cr 37% at TR 1700 ms compared with other TR, and also signal increased at $0.3mmol/{\ell}$, In $0.5mmol/{\ell}$ of contrast agent, cerebral metabolite peaks reduced, especially when TR 1500 ms and 2000 ms they decreased below those of control group. The ratio of metabolite peaks such as NAA/Cr and Cho/Cr decreased as the concentration of the contrast agent increased from 0.1 to $0.5mmol/{\ell}$. Authors found that the optimization of PRESS sequence for 0.3T MRS was as follows: low density of contrast agent ($0.1mmol/{\ell}$ and $0.3mmol/{\ell}$) made the highest signal intensity, while high density of contrast agent reveals the least reduction of signal intensity at 1700 ms. In conclusion, authors believe that it is helpful to reduce TR for acquiring maximum signal intensity.

A Microsporidian Parasite - $Lb_{ms}$ (Protozoa - Microspora) Infecting Lamerin Breed of the Silkworm Bombyx mori L. (Lepidoptera - Bombycidae)

  • Bhat Shabir Ahmad;Nataraju B.
    • International Journal of Industrial Entomology and Biomaterials
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    • v.12 no.1
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    • pp.41-43
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    • 2006
  • Lamerin breed of the silkworm Bombyx mori L. is the only mulberry silkworm breed which survives with an associated microsporidian $(Lb_{ms})$ infection from generations. This present comparative investigation has produced information on the influence of $Lb_{ms}$ on the growth and development of the breed. The $Lb_{ms}$ transmits tranovarially as well as perorally at low level. Larvae developed from the eggs laid by female, infected with $Lb_{ms}$ were as normal as larvae developed from the eggs laid by healthy female. In infected tissues early developmental stages and mature spores located intracellularly but did not show hypertrophy of cells of the host. The meronts and sporonts measures $0.46{\pm}0.25,\;1.11{\pm}0.05{\mu}m$ in length and $0.32{\pm}0.05,\;0.78{\pm}0.10{\mu}m$ in width respectively. The mature spore measures $4.36{\pm}0.06{\mu}m$ in length and $2.14{\pm}0.01{\mu}m$ in width.