• Title/Summary/Keyword: ion detection

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Identification and evaluation of fragmentation pathways of PDE-5 inhibitor analogues using LC-QTOF-MS (LC-QTOF-MS를 이용한 발기부전치료제 유사물질의 fragmentation pathway 분석)

  • Do, Jung-Ah;Noh, Eunyoung;Yoon, Soon-Byung;Park, Hyoung-Joon;Cho, Sooyeul;Park, Sung-Kwan;Yoon, Chang-Yong
    • Analytical Science and Technology
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    • v.28 no.4
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    • pp.278-287
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    • 2015
  • Phosphodiesterase type 5 inhibitors (PDE-5 inhibitors) are used in the treatment of erectile dysfunction. In recent years, a number of reports have been conducted on dietary supplements contaminated with PDE-5 analogues. In this study, 58 analogues of PDE-5 inhibitors were sorted into five groups: tadalafil, sildenafil, hongdenafil, vardenafil, and other analogues. These analogues were then evaluated using a liquid chromatography-quadrupole-time of flight mass spectrometry (LC-QTOF-MS) electrospray ionization mass method. Each compound has a unique fragmentation ion, which can be easily analyzed qualitatively. The fragmentation pathways of the analogues were elucidated based on the QTOF-MS and MS/MS data. Common ions were confirmed for each group by analyzing the structural characteristics and fragmentation pathways. Specifically, common ions were observed at m/z 169.08 and 135.04 (tadalafil analogues), m/z 311.15 and 283.12 (sildenafil analogues and hongdenafil analogues), and m/z 312.16 and 151.09 (vardenafil analogues). The advantage of this method is that the structure of unknown components can be determined by interpreting the product ions. Hence, the developed method can be used for the identification of unknown compounds. Fragmentation pathways may also aid in the detection and identification of PDE-5 inhibitor analogues.

Development of Rapid Analysis Method for Pesticide Residues by GC-MS/MS (GC-MS/MS를 이용한 잔류농약 신속검사법 개발)

  • Choi, Yong-Hoon;Nam, Hye-Seon;Hong, Hye-Mi;Lee, Jin-Ha;Chae, Kab-Ryong;Lee, Jong-Ok;Kim, Hee-Yun;Yoon, Sang-Hyeon
    • The Korean Journal of Pesticide Science
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    • v.9 no.4
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    • pp.292-302
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    • 2005
  • Condition of Ion-Trap gas chromatography-mass spectrometry (GC-MS) for rapid screening of 206-pesticides residues in agricultural foodstuffs was optimized. As applying a wide-bore column (10 m${\times}$0.53 mm, DF 0.25 um) connected with a fused silica restrictor (0.6 m${\times}$0.1 mm), a significant retention time reduction was obtained. Additionally, the shape of peaks was sharper and higher than classical GC's and GC-MS's, which allowed lower detection limits. To easily manage many spectral data, both of Electron Ionization(EI) and Chemical Ionization(CI) techniques were adopted in screening procedure. At the following steps, MS-MS technique were used to confirm screened analytes in complicated matrices.

Studies on the Activity and Stability of Egg White lysozyme (난백 lysozyme의 역가측정과 안정성에 관한 연구)

  • 이성기;유익종;김기성;김영붕
    • Korean Journal of Poultry Science
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    • v.17 no.2
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    • pp.109-114
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    • 1990
  • Enzymatic activity of isolated Lysozyme from egg white by cation ion-exchange chromatography was detected with various methods and stability of lysozyme in solution was studied by heat and pH treatments. Lysozyme activity refered to mg pure lysozyme/mg sample was more accurate although it needed standard lysozyme. But lysozyme activity refered to units/mg sample could be detected easily and reducted total detection time. Enzymatic activity of isolated lysozyme which dissolved in 0.066M phosphate buffer(pH 6.3) and then incubated at $37^{\circ}C$ for 2hr was increased remarkably on the lysis of Micrococcus lysodeikticus. The activity of isolated lysozyme by CM Sephadex C-25 was higher in eluting solution of above O. D. 1.0 at 640nm and attained 36, 000 units/mg solid. The stability of isolated lysozyme was decreased by various heat treatment. Activity began to decrease above 6$0^{\circ}C$ and dropped rapidly at $100^{\circ}C$. Especially, 35% loss of activity occured in 0.066M phosphate buffer at $100^{\circ}C$. for 15min. The stability of lysozyme was also affected by pH. lysozyme was very stable in acidic solution but in alkaline solution. Enzymatic activity showed maximum value at pH 3.0 solution while decreased rapidly above pH 6.0 solution.

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Influence of Ammonium Phosphate on Mycelial Morphology during Submerged Cultivation of Ganoderma lucidum (영지의 액체배양에 있어서 균사체 형태에 미치는 Ammonium Phosphate의 영향)

  • Lee, Kyu-Min;Lee, Shin-Young
    • The Korean Journal of Mycology
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    • v.29 no.2
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    • pp.91-98
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    • 2001
  • The mycelial morphology during submerged cultivation of Ganoderma ludium using by air-lift fermenter system were analyzed by image processing system and the characterization of mycelial morphology were investigated. In submerged culture using medium with different ammonium phosphate concentrations, the various morphological forms of G. lucidum mycelium were observed. The filamentous forms such as non-branched long filamentous mycelium, non-branched short mycelium, branched long filamentous mycelium, branched short mycelium, entangled mycelium and clump were observed, and also, and also, the pelleted forms such as smooth pellet, rough pellet and hollow rough pellet were observed. The mycelial morphology was changed from the filamentous to the pelleted forms by addition of ammonium phosphate. The fractal dimensions of pelleted and filamentous forms were 1.05 and 1.3, respectively, while the fractal dimension of mixtures of pelleted and filamentous forms was 1.16. Therefore, the fractal dimension was found to be more effective index for the detection of the mycelial morphology and morphological change during batch cultivation. The circularity was also found to be useful for evaluating the surface growth of pelleted mycelium.

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Analytical Determination of Cyanide in Maesil (Prunus mume) Extracts (매실추출제품의 시안화합물 분석법에 관한 연구)

  • Kim, Eun-Jung;Lee, Hwee-Jae;Jang, Jin-Wook;Kim, In-Young;Kim, Do-Hyeong;Kim, Hyun-Ah;Lee, Soo-Min;Jang, Ho-Won;Kim, Sang-Yub;Jang, Young-Mi;Im, Dong-Kil;Lee, Sun-Hee
    • Korean Journal of Food Science and Technology
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    • v.42 no.2
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    • pp.130-135
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    • 2010
  • Picrate, enzyme-picrate and instrumental analysis methods using IC (Ion Chromatography) and HPLC (High Performance Liquid Chromatography) were compared for their effectiveness in determining cyanide in extracts of Maesil, which is classified as a harmful substance. First, the picrate method showed the shortest analysis time (about 5 hr). The color of picrate paper changed at 0.01 mg/$200\;mL\;CN^-$. However, it was difficult to detect cyanide from amygdalin of glucosides. Second, we performed a qualitative analysis for total cyanide (free cyanide and cyanide from amygdalin) by the enzyme-picrate method using $\beta$-glucosidase and a quantitative analysis by spectrophotometry. Finally, analysis of cyanide by IC and HPLC required the longest determining time (about 17 hr) as well as pretreatment for each free cyanide and amygdalin. These results suggest that enzyme-picrate is the most effective analysis method for the detection of cyanide in Maesil extracts.

Development of an Official Method for Measurement of Fluazinam Residues for Quarantine of Imported and Exported Horticultural Products (수출입 원예작물의 검역을 위한 살균제 Fluazinam의 공정 잔류분석법 개발)

  • Kim, Gyeong-Ha;Ahn, Kyung-Geun;Kim, Gi-Ppeum;Hwang, Young-Sun;Chang, Moon-Ik;Kang, In-Kyu;Lee, Young Deuk;Choung, Myoung-Gun
    • Horticultural Science & Technology
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    • v.34 no.1
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    • pp.183-194
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    • 2016
  • This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was $0.004mg{\cdot}kg^{-1}$ in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.

Production and Characterization of vitellogenin monoclonal antibody on the Scorpion fish Sebastiscus marmoratus (쏨뱅이, Sebastiscus marmoratus의 vitellogenin 단클론 항체생산 및 특성에 관한 연구)

  • Kim, Young-Ju;Lim, Yoon-Kyu;Yeo, In-Kyu
    • Journal of fish pathology
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    • v.26 no.3
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    • pp.241-254
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    • 2013
  • In order to establish bio-marker systems for the screening of endocrine-disrupting chemicals contaminated in various environment, Vitellogenin(Vtg) bio-marker have been developed to detect Scorpion fish's(Sebastiscus marmoratus) Vtg. Vtg has been induced by administration of estradiol into S. marmoratus, and purified by gel filtration and ion-exchange chromatography from serum of the fish. After immunization of the purified Vtg into BALB/c mouse, hybridomas secreting anti-Vtg antibodies have been produced. The size of induced Vtg in the serum was about 440 kDa by gel filtration using Sepharose CL-6B. By SDS-PAGE analysis, the main band of Vtg, however, was at 175 kDa, and several minor bands have been detected with the main band. Eight different monoclonal antibodies have been produced from established hybridomas and the antibodies did not cross-react with sera from different species of fishes tested in this study except with that of Sebastes hubbsi. These results suggested that the monoclonal antibody of S28 and S15 can used as capture and tracer antibodies for ELISA and ICG assays. The detection systems developed in this study can be used as Bio-marker assays to check endocrine disrupting activity of various chemicals as well as to detect known endocrine disrupting chemicals contaminated in environment.

Analytical Methods for Diethylstibestrol and Zeranol in Muscle Foods (근육 식품 중의 diethylstibestrol과 zeranol 분석법)

  • Ha, Jae-Ho
    • Korean Journal of Food Science and Technology
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    • v.34 no.3
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    • pp.385-389
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    • 2002
  • Analytical method for diethylstibestrol (DES) and zeranol, which are growth promoters, in muscle foods was studied. Through selected ion monitoring analysis by GC-MSD for hormones, $M^+$ 412, 420, 416, and 433 for DES, $D_8DES$, ${\beta}-estradiol$, and zeranol, respectively, were selected for quantitative analysis. Removal of interferences in meat was done by passing the meat through 1 cc of strong anion exchanges resin, Dowex $2{\times}8$, 400 mesh, whereby the recoveries of DES and zeranol were achieved. Recoveries of DES and zeranol were ranged from 85 to 110%, and 75 to 110%, respectively, in meat using $D_8DES$ as an internal standard, while were 82 to 105%, and 65 to 120%, respectively, using ${\beta}-estradiol$ as an internal standard. These results show that both $D_8DES$ and ${\beta}-estradiol$ can be adopted as the internal standard for the analysis of DES and zeranol in muscle foods. Limits of detection of DES and zeranol were 0.05 and 1.0 ng/g, and limits of quantitation were 0.5 and 1.0 ng/g, respectively. The results of this study revealed no DES and zeranol were present in 14 samples of beefs, porks, ducks, chickens, mutiplicated flat fish, and trout.

Development of Simultaneous Analysis of Ferulic Acid, Caffeic Acid, Catechin and Taxifolin from Health Functional Food Pinus Pinaster Bark Extract by UPLC-MS/MS (건강기능식품 프랑스해안송껍질추출물 중 UPLC-MS/MS를 이용한 Ferulic acid, Caffeic acid, Catechin, Taxifolin 동시분석법 개발 연구)

  • Oh, Jae-Myoung;Kim, Ji An;Hu, Soo Jung;Choi, Yoon Hee;Oh, Keum Soon
    • Journal of Food Hygiene and Safety
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    • v.34 no.5
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    • pp.431-437
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    • 2019
  • This study was conducted to develop a simultaneous analysis method for ferulic acid, caffeic acid, catechin and taxifolin from Health Functional Food (HFF) Pinus Pinaster bark extract. The simultaneous analytical method for ferulic acid, caffeic acid, catechin and taxifolin is carried out using UPLC-MS/MS. The method validation was performed to determine selectivity, linearity, accuracy, limit of detection (LOD), limit of quantification (LOQ) and precision for ferulic acid, caffeic acid, catechin and taxifolin. LC-MS/MS method was established using an Acquity UPLC BEH $C_{18}$ Column and was applied for these 4 compounds. Product-ion traces, at m/z $194.2{\rightarrow}133$, $180.2{\rightarrow}135$, $290.3{\rightarrow}245$, $304.3{\rightarrow}248$, were used for quantitative analysis of ferulic acid, caffeic acid, catechin and taxifolin, respectively. Excellent linearity ($r^2=0.999$) was observed for ferulic acid, caffeic acid, catechin and taxifolin in the concentration range (50-2500 mg/L). The observed recoveries of these 4 compounds were found to be between 84.9 and 104.9%, while precision was between 1.20 and 4.43% relative standard deviation (% RSD).

Characteristics of OCP of Reinforced Concrete Using Socket-type Electrodes during Periodic Salt Damage Test (주기적 염해 시험에 따른 소켓 타입 전극을 활용한 철근 콘크리트의 OCP 특성)

  • Lee, Sang-Seok;Kwon, Seung-Jun
    • Journal of the Korea institute for structural maintenance and inspection
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    • v.25 no.4
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    • pp.28-36
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    • 2021
  • It is known that buried rebars inside concrete structures are protected from corrosion due to passive layer. It is very important to delay the timing of corrosion or evaluate a detection of corrosion initiation for the purpose of cost-beneficiary service life of a structure. In this study, corrosion monitoring was performed on concrete specimens considering 3 levels of cover depth(60 mm, 45 mm, and 30 mm), W/C(water to cement) ratio(40.0%, 50.0%, and 60.0%) and chloride concentration(0.0%, 3.5%, and 7.0%). OCP(Open Circuit Potential) was measured using agar-based socket type sensors. The OCP measurement showed the consistent behavior where the potential was reduced in wet conditions and it was partially recovered in dry conditions. In the case of 30 mm of cover depth for most W/C ratio cases, the lowest OCP value was measured and rapid OCP recovery was evaluated in increasing cover depth from 30 mm to 45 mm, since cover depth was an effective protection against chloride ion ingress. As the chloride concentration increased, the effect on the cover depth tended to be more dominant than the that of W/C ratio. After additional monitoring and physical evaluation of chloride concentration after specimen dismantling, the proposed system can be improved with increasing reliability of the corrosion monitoring.