• Title/Summary/Keyword: Ionization development

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Quantification of Three Prohibited Anabolic-Androgenic Steroids in Equine Urine using Gas Chromatography-Tandem Mass Spectrometry

  • Young Beom Kwak;Shaheed Ur Rehman;Hye Hyun, Yoo
    • Mass Spectrometry Letters
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    • v.14 no.3
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    • pp.104-109
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    • 2023
  • Anabolic-androgenic steroids (AAS) are used illegally to enhance muscle development and increase strength and power. In this study, a reliable, and sensitive quantitative method was developed and validated using heptafluorobutyric acid anhydride (HFPA) derivatives for the simultaneous detection of prohibited AAS (testosterone [TS], boldenone [BD], 5α-estrane-3β,17α-diol [EAD]) using gas chromatography-tandem mass spectrometry (GC-MS/MS). For processing the samples, solid phase extraction, methanolic hydrolysis, and liquid-liquid extraction were used. For detection using mass spectrometry, the multiple reaction monitoring (MRM) mode was used with the electron ionization (EI) positive mode. The method was evaluated for selectivity, linearity, lower limit of quantification, intra- and inter-day precision, accuracy, and stability. The results showed that the method was accurate and reproducible for the quantitation of the three steroids. The developed method was finally applied to the analysis of a suspect gelding urine sample received from the Asian Quality Assurance Program (AQAP).

Analysis of Marker Substances in Samul-tang by HPLC-MS/MS (HPLC-MS/MS에 의한 사물탕의 지표성분 분석)

  • Yu, Young-Beob;Kim, Mi-Jung;Huang, Dae-Sun;Ha, Hye-Kyeong;Ma, Jin-Yeul;Shin, Hyeun-Kyoo
    • The Korea Journal of Herbology
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    • v.22 no.2
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    • pp.97-102
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    • 2007
  • Objectives : This study presents a high performance liquid chromatography - electrospray ionization-mass spectrometer (HPLC-MS/MS) methods for the quantitative and qualitative analysis of various active components in Samul-tang, which is composed of four crude herbs. Methods : HPLC-ESI-MS/MS for the determinations of paeoniflorin and 5-HMF (5-hydroxymethyl 2-furaldehyde) in the Samul-tang, the separation method was performed on an COSMOS1L 5C18-AR-Il (2.0 X 150 mm I.D.) column by gradient elution with 0.1% acetic acid and 5% CH3CN in water (A)-0.1% acetic acid and 5% H20 in CH3CN (B) as the mobile phase at a flow-rate of 300 ${\mu}L/min$ with detection at quadrupole mass spectrometer. The all marker substances were always detected as the base peaks in the positive ion mode. Results : The paeoniflorin of Paeoniae Radix in Samul-tang showed a strong base peak [M+H2O]+ in the positive detection mode to give the following as; paeoniflorin (498.109 [M+H2O]+, 479.8 [M]+, 301 [M-glucose]+, 179.3 [glucose]+). Based on the HPLC retnetion time and MS of standard compounds confirmed the identity of active compounds in Rehmanniae Radix Preparata as follows; 5-HMF (127.0[M+H]+, 109.3 [M-OH]+) in the positive ion mode. Conclusion : According to the above results, HPLC-ESI-MS method permits assignment of tentative structures such as paeoniflorin and 5-HMF in the Samul-tang.

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Quantitative Analysis of Cinnamaldehyde, Cinnamylalcohol and Salicylaldehyde in Commercial Biopesticides Containing Cinnamon Extract Using Gas Chromatography - Flame Ionization Detector

  • Lim, Sung-Jin;Lee, Ji-Hye;Kim, Jin-Hyo;Choi, Geun-Hyoung;Cho, Nam-Jun;Park, Byung-Jun
    • Korean Journal of Environmental Agriculture
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    • v.33 no.3
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    • pp.213-219
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    • 2014
  • BACKGROUND: In an environment-friendly agriculture, plant extracts have been perceived as alternatives of synthetic pesticides. The Environment-friendly Agriculture Promotion Act of Korea has approved cinnamon extract as a matter for the production of commercial biopesticides. Thirteen commercial biopesticides containing cinnamon extract have been marketed locally. However, the analytical method for the quality control of these biopesticides containing cinnamon extract has not been studied. METHODS AND RESULTS: Cartridge clean-up method for the determination of cinnamaldehyde, cinnamylalcohol and salicylaldehyde in biopesticides containing cinnamon extract was developed and validated by gas chromatography (GC). The clean-up method was optimized with HLB SPE cartridges for the bioactive substance in biopesticides containing cinnamon extract, and the eluate was analyzed by GC. The developed method was validated, and the LOQ and recovery rates of cinnamaldehyde, cinnamylalcohol and salicylaldehyde were 0.139, 0.067 and $0.062mgL^{-1}$ and 84.2, 86.5 and 82.1%, respectively. The contents of cinnamaldehyde, cinnamylalcohol and salicylaldehyde were analyzed using the developed method in the 13 commercial biopesticides. Results showed 0.06-17.37%,

A New Analytical Method for Erythromycin in Fish by Liquid Chromatography/Tandem Mass Spectrometry

  • Park, Mi-Jung;Park, Mi-Seon;Lee, Tae-Seek;Shin, Il-Shik
    • Food Science and Biotechnology
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    • v.17 no.3
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    • pp.508-513
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    • 2008
  • Erythromycin has been used to treat Streptococosis, Edwardsiel1osis, Vibriosis, Bacterial enteritis in the cultured fish. In this study, a rapid and effective erythromycin analysis method with new sample treatment protocol and liquid chromatography/tandem mass spectrometry (LC/MS/MS) system for fish products was developed. For the erythromycin extraction from fish muscle, the solvent mixture composed of 0.2% meta-phosphoric acid and methanol (6:4) showed good recovery rate, and the optimum extraction solvent volume was 20 mL. Erythromycin detection using LC/MS/MS were carried out under electro spray ionization (ESI) positive condition and erythromycin mass value 576.2 and 157.9. And the detection limit of the established method was 0.005 mg/kg in fish products. The recovery rate of the developed method applied to the fish species were as following, olive flounder, $87.6{\pm}5.0%$; black rockfish, $87.2{\pm}6.4%$; eel, $85.2{\pm}4.8%$; and rainbow trout, $86.0{\pm}6.2%$. In the established method in this study, the correlation of coefficient values ($R^2$) of erythromycin calibration curve (n=11) was 0.9998.

Trends in Broadband Terahertz Detector Technology (광대역 테라헤르츠 검출 소자 기술 동향)

  • Shin, J.H.;Choi, D.H.;Lee, E.S.;Moon, K.W.;Park, D.W.;Joo, K.I.;Kim, M.G.;Choi, K.S.;Lee, I.M.;Park, K.H.
    • Electronics and Telecommunications Trends
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    • v.35 no.4
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    • pp.53-64
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    • 2020
  • The terahertz (THz) region lies in between the millimeter and infrared spectral bands. A THz wave has the characteristics of non-invasiveness and non-ionization due to low photon energies, while having high penetrability in dielectrics. In addition, since the resonance frequencies of various molecules are included in the THz band, research on the application of spectral analysis and non-destructive testing has been widely studied. Towards this end, the research and development of THz detectors has become increasingly important in order to assess their applications in different areas such as astronomy, security, industrial non-destructive evaluations, biological applications, and wireless communications. In this report, we summarize the operating principles, characteristics, and utilization of various broadband technologies in THz detection devices. Further, we introduce the development status of our Schottky barrier diode technology as one of the broadband THz detectors that can be easily adopted as direct detectors in many fields of applications.

Understanding radiation effects in SRAM-based field programmable gate arrays for implementing instrumentation and control systems of nuclear power plants

  • Nidhin, T.S.;Bhattacharyya, Anindya;Behera, R.P.;Jayanthi, T.;Velusamy, K.
    • Nuclear Engineering and Technology
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    • v.49 no.8
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    • pp.1589-1599
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    • 2017
  • Field programmable gate arrays (FPGAs) are getting more attention in safety-related and safety-critical application development of nuclear power plant instrumentation and control systems. The high logic density and advancements in architectural features make static random access memory (SRAM)-based FPGAs suitable for complex design implementations. Devices deployed in the nuclear environment face radiation particle strike that causes transient and permanent failures. The major reasons for failures are total ionization dose effects, displacement damage dose effects, and single event effects. Different from the case of space applications, soft errors are the major concern in terrestrial applications. In this article, a review of radiation effects on FPGAs is presented, especially soft errors in SRAM-based FPGAs. Single event upset (SEU) shows a high probability of error in the dependable application development in FPGAs. This survey covers the main sources of radiation and its effects on FPGAs, with emphasis on SEUs as well as on the measurement of radiation upset sensitivity and irradiation experimental results at various facilities. This article also presents a comparison between the major SEU mitigation techniques in the configuration memory and user logics of SRAM-based FPGAs.

Quantitative Determination of Ascaridole, Carvacrol and p-Cymene in the Biopesticides Products Derived from Chenopodium ambrosioides L. Extracts by Gas Chromatography

  • Yang, Ji-Yeon;Ryu, Song-Hee;Lim, Sung-Jin;Choi, Geun-Hyoung;Park, Byung-Jun
    • Korean Journal of Environmental Agriculture
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    • v.35 no.3
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    • pp.211-215
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    • 2016
  • BACKGROUND: The commercial biopesticides containing Chenopodium ambrosioides L. extracts which have been registered as one of the ingredients of the commercial biopesticide by the organic agriculture materials, and have been widely used in Republic of Korea. However, the quantitative analysis method of the active substances for the commercial biopesticides containing C. ambrosioides L. extract has not been conducted.METHODS AND RESULTS: To analyze the quantitative analysis of ascaridole, carvacrol, and p-cymene as active substances of C. ambrosioides L. extract, hydrophilic lipophilic balance cartridge was used for solid phase extraction. The active substances were analyzed by the gas chromatography with flame ionization detector. The limit of quantitation values of ascaridole, carvacrol, and p-cymene were 10, 5, and 2 mg/L, and the recovery rates were 96.3, 84.0, and 82.5% in liquid products and 98.3, 99.1, and 97.3% in solid products, respectively. The total content of ascaridole, carvacrol, and p-cymene in the commercial biopesticides was ranged from 0.08 to 12.75%.CONCLUSION: From these results, this method was suitable for the quantitative analysis of the active substances of commercial biopesticides containing C. ambrosioides L. extract.

Determination of Residual Erythromycin Antibiotic in Fishery Products by Liquid Chromatography-electrospray Ionization Mass Spectrometry (LC-MS/MS를 이용한 어류 및 갑각류의 잔류 Erythromycin 항생제 분석)

  • Jo, Mi-Ra;Mok, Jong-Soo;Lee, Doo-Seog;Kim, Min-Jung;Kim, Poong-Ho
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.42 no.1
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    • pp.15-19
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    • 2009
  • A simple and sensitive method for erythromycin quantification by liquid chromatography electrospray mass spectrometry (LC-MS/MS) in fishery products was developed. Samples were extracted by liquid-liquid extraction using 70% acetonitrile. Lipids were removed by acetonitrile saturated hexane. LC separation was performed on a Shiseido UG C-18 column ($150\;mm{\times}2.0\;mm$ internal diameter.) with a gradient system of 0.2% acetic acid-acetonitrile containing 0.2% acetic acid as a mobile phase at flow rate of 0.2 mL/min. The mass spectrometer was operated in selected reaction monitoring with positive electro-spray interface. Transitions were monitored a m/z $734{\to}577$ and $734{\to}158$, with m/z $734{\to}577$ chosen for quantification. Recovery of erythromycin from fish and shrimp fortified at the 10 ng/mL, 50 ng/mL and 100 ng/mL were 91.6-109.4%, 84.4-111.2% and 98.8-109.6% with high precision, respectively. Limits of quantification and limits of detection of erythromycin in both fish and shrimp were 10.0 ng/mL and 1.0 ng/mL, respectively. This analysis method for erythromycin has been proposed for registration in the Korean Official Methods of Food Analysis and has been utilized for fishery products analysis by the Korea Food and Drug Adminstration and the National Fisheries Products Quality Inspection Service.

The Antibiosis Action and Rice-Induced Resistance, Mediated by a Lipopeptide from Bacillus amyloliquefaciens B014, in Controlling Rice Disease Caused by Xanthomonas oryzae pv. oryzae

  • Li, Shu Bin;Xu, Shi Ru;Zhang, Rui Ning;Liu, Yuan;Zhou, Ren Chao
    • Journal of Microbiology and Biotechnology
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    • v.26 no.4
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    • pp.748-756
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    • 2016
  • In the present study, a lipopeptide (named AXLP14) antagonistic to Xanthomonas oryzae pv. oryzae (Xoo) was obtained from the culture supernatant of Bacillus amyloliquefaciens B014. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry analysis demonstrated that AXLP14 consisted of surfactin homologs. The minimum inhibition concentration and minimum bactericidal concentration of AXLP14 against Xoo were determined to be 1.25 and 2.50 mg/ml, respectively. At a concentration of 0.613 mg/ml, AXLP14 strongly inhibited the formation of Xoo biofilm. AXLP14 also inhibited the motility of Xoo in a concentration-dependent manner. Applying AXLP14 to rice seedlings significantly reduced the incidence and severity of disease caused by Xoo. In Xoo-infected rice seedlings, AXLP14 strongly and continuously up-regulated the expression of both OsNPR1 and OsWRKY45. In addition, AXLP14 effectively inhibited the Xoo-induced up-regulation of the expression of the abscisic acid biosynthesis gene OsNECD3 and the abscisic acid signalingresponsive gene OsLip9, indicating that AXLP14 may protect rice against Xoo-induced disease by enhancing salicylic acid defense and interfering with the abscisic acid response to virulence.

Feasibility Study for Development of Transit Dosimetry Based Patient Dose Verification System Using the Glass Dosimeter (유리선량계를 이용한 투과선량 기반 환자선량 평가 시스템 개발을 위한 가능성 연구)

  • Jeong, Seonghoon;Yoon, Myonggeun;Kim, Dong Wook;Chung, Weon Kuu;Chung, Mijoo;Choi, Sang Hyoun
    • Progress in Medical Physics
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    • v.26 no.4
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    • pp.241-249
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    • 2015
  • As radiation therapy is one of three major cancer treatment methods, many cancer patients get radiation therapy. To exposure as much radiation to cancer while normal tissues near tumor get little radiation, medical physicists make a radiotherapy plan treatment and perform quality assurance before patient treatment. Despite these efforts, unintended medical accidents can occur by some errors. In order to solve the problem, patient internal dose reconstruction methods by measuring transit dose are suggested. As feasibility study for development of patient dose verification system, inverse square law, percentage depth dose and scatter factor are used to calculate dose in the water-equivalent homogeneous phantom. As a calibration results of ionization chamber and glass dosimeter to transit radiation, signals of glass dosimeter are 0.824 times at 6 MV and 0.736 times at 10 MV compared to dose measured by ionization chamber. Average scatter factor is 1.4 and Mayneord F factor was used to apply percentage depth dose data. When we verified the algorithm using the water-equivalent homogeneous phantom, maximum error was 1.65%.