• 제목/요약/키워드: Background ions

검색결과 73건 처리시간 0.03초

액체크로마토그래프-질량분석기를 이용한 정성 및 정량 오류의 확인 (Identification of Pitfalls Related to the Analysis of Liquid Chromatography-Tandem Mass Spectrometry and Liquid Chromatography-Time of Flight Mass Spectrometry)

  • 권진욱;조윤제;이규식
    • 한국환경농학회지
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    • 제34권3호
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    • pp.230-237
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    • 2015
  • BACKGROUND: To identify the sources of inaccuracy in LC/MS/MS methods used in the routine quantitation of small molecules are described and discussed. METHODS AND RESULTS: Various UPLC coupled to triple quadrupole mass spectrometer and time of flight (TOF) were used to identify the potential sources of inaccuracy and inducing the pitfalls of qualification and quntitation during the veterinary drug residue analysis. Some of stable isotope labelled veterinary drugs, which were used as internal standards, presented "cross-talk", regardless of manufactures of mass spectrometer and types of spectrometer. Group of sulfonamides also presented inaccuracy qualification and quantitation due to the multi-residue analytical method with the same fragment ions at the close retention times. CONCLUSION: The phenomena of "cross-talk" occurring between subsequently monitored transition from stable isotope labelled and isotope non-labelled authentic chemical were identified. To prevent errors and achieve more accurate data during the analysis of small molecules by LC/MS/MS SRM method, Followings should be taken care of and kept checking; purity and concentration of stable isotope as an internal standard, prevention of carry-over during the separation in column, minimizing the ion suppression by matrix effect, identification of retention time, precursor ion and product ion, and full knowledge of data processing including smoothing and peak integration.

Excessive copper in feed not merely undermines animal health but affects food safety

  • Ma, Zicheng;Li, Yan;Han, Zifeng;Liu, Zhaohu;Wang, Hongyu;Meng, Fanliang;Liu, Sidang;Chen, Dawei;Liu, Mengda
    • Journal of Veterinary Science
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    • 제22권3호
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    • pp.31.1-31.12
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    • 2021
  • Background: Blackened intestines in slaughtered pigs have been commonly observed in China in recent years. However, no cause has been reported. Objectives: We attempted to determine whether the blackening of the pig intestine was related to an excess of copper (Cu) in their feed. Methods: In this study, we observed and collected porcine intestines in small- and large-scale pig slaughterhouses in Shandong province from May to October 2018. Twelve types of metal ions were detected in the black intestinal samples. Results: The Cu level in the intestine samples was mostly higher than the Chinese national limit for food. Further study showed that Cu supplementation in most commercial porcine feed also exceeded the national standard. An animal model (mouse) that could mimic the intestinal blackening in pigs was established. Compared to control mice, Cu accumulated in the liver and intestines of mice fed an excessive Cu level, confirming the excessive Cu in the feed may be considered the major cause of blackened porcine intestines. Microscopic examination revealed that black intestines had many particles containing Cu in the lamina propria of the intestinal mucosa, and the intestinal mucosal epithelial cells showed degeneration and necrosis. Conclusions: In conclusion, overuse of Cu in animal feed can lead to animal poisoning and Cu accumulation in animal products. Such overuse not only harms the health of livestock but can also affect public health.

Differentiation and identification of ginsenoside structural isomers by two-dimensional mass spectrometry combined with statistical analysis

  • Xiu, Yang;Ma, Li;Zhao, Huanxi;Sun, Xiuli;Li, Xue;Liu, Shuying
    • Journal of Ginseng Research
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    • 제43권3호
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    • pp.368-376
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    • 2019
  • Background: In the current phytochemical research on ginseng, the differentiation and structural identification of ginsenosides isomers remain challenging. In this paper, a two-dimensional mass spectrometry (2D-MS) method was developed and combined with statistical analysis for the direct differentiation, identification, and relative quantification of protopanaxadiol (PPD)-type ginsenoside isomers. Methods: Collision-induced dissociation was performed at successive collision energy values to produce distinct profiles of the intensity fraction (IF) and ratio of intensity (RI) of the fragment ions. To amplify the differences in tandem mass spectra between isomers, IF and RI were plotted against collision energy. The resulting data distributions were then used to obtain the parameters of the fitted curves, which were used to evaluate the statistical significance of the differences between these distributions via the unpaired t test. Results: A triplet and two pairs of PPD-type ginsenoside isomers were differentiated and identified by their distinct IF and RI distributions. In addition, the fragmentation preference of PPD-type ginsenosides was determined on the basis of the activation energy. The developed 2D-MS method was also extended to quantitatively determine the molar composition of ginsenoside isomers in mixtures of biotransformation products. Conclusion: In comparison with conventional mass spectrometry methods, 2D-MS provides more direct insights into the subtle structural differences between isomers and can be used as an alternative approach for the differentiation of isomeric ginsenosides and natural products.

Calcium release and physical properties of modified carbonate apatite cement as pulp capping agent in dental application

  • Zakaria, Myrna Nurlatifah;Cahyanto, Arief;El-Ghannam, Ahmed
    • 생체재료학회지
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    • 제22권4호
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    • pp.346-351
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    • 2018
  • Background: Carbonate apatite ($CO_3Ap$) and silica-calcium phosphate composite (SCPC) are bone substitutes with good prospect for dental application. SCPC creates a hydroxyapatite surface layer and stimulate bone cell function while, $CO_3Ap$ induce apatite crystal formation with good adaptation providing good seal between cement and the bone. Together, these materials will add favorable properties as a pulp capping material to stimulate mineral barrier and maintain pulp vitality. The aim of this study is to investigate modification of $CO_3Ap$ cement combined with SCPC, later term as $CO_3Ap-SCPC$ cement (CAS) in means of its chemical (Calcium release) and physical properties (setting time, DTS and pH value). Methods: The study consist of three groups; group 1 (100% calcium hydroxide, group 2 $CO_3Ap$ (60% DCPA: 40% vaterite, and group 3 CAS (60% DCPA: 20% vaterite: 20% SCPC. Distilled water was employed as a solution for group 1, and $0.2mol/L\;Na_3PO_4$ used for group 2 and group 3. Samples were evaluated with respect to important properties for pulp capping application such as pH, setting time, mechanical strength and calcium release evaluation. Results: The fastest setting time was in $CO_3Ap$ cement group without SCPC, while the addition of 20% SCPC slightly increase the pH value but did not improved the cement mechanical strength, however, the mechanical strength of both $CO_3Ap$ groups were significantly higher than calcium hydroxide. All three groups released calcium ions and had alkaline pH. Highest pH level, as well as calcium released level, was in the control group. Conclusion: The CAS cement had good mechanical and acceptable chemical properties for pulp capping application compared to calcium hydroxide as a gold standard. However, improvements and in vivo studies are to be carried out with the further development of this material.

Comparison of the bovine blood gas parameters produced with three types of portable blood gas analyzers

  • Ro, Younghye;Choi, Woojae;Hong, Leegon;Kim, Eunkyung;Choe, Eunhui;Kim, Danil
    • Journal of Veterinary Science
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    • 제23권4호
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    • pp.60.1-60.6
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    • 2022
  • Background: A definite diagnosis should be made in the bovine practice field, however, it was difficult to perform laboratory analysis immediately. Currently, three types of portable blood gas analyzers are available in Korea. Objectives: This study aimed to evaluate the correlations among these three analyzers. Methods: Seventy-two plasma samples from Holstein-Friesian cows were used for blood gas analysis, and three instruments (EDAN i15 Vet, VETSCAN i-STAT, and EPOC) were operated simultaneously. Moreover, plasma calcium levels were compared between these portable analyzers and blood chemistry device, which is usually used in a laboratory environment. Pearson analysis was performed to confirm the correlation of each parameter produced with the three instruments and blood chemistry analyzer. Results: As results, high correlation was observed in parameters of pH, pO2, potassium ion, ionized calcium, and glucose (p < 0.001, r > 0.7). In addition, pCO2 showed a moderate correlation among the three analyzers (p < 0.001, r > 0.5), and there was no correlation among all instruments for sodium ions. There was also a high correlation between ionized calcium from the three portable devices and total calcium from the biochemistry analyzer (p < 0.001, r > 0.9). Conclusions: In conclusion, there was a high correlation between results from the three different blood gas analyzers used in the bovine clinical field in Korea. Thus, a consistent diagnosis can be made even with different equipment if the operator is aware of the strengths and weaknesses of each piece of equipment and operates it properly.

Suppression of stray electrons in the negative ion accelerator of CRAFT NNBI test facility

  • Yuwen Yang ;Jianglong Wei ;Junwei Xie ;Yuming Gu;Yahong Xie ;Chundong Hu
    • Nuclear Engineering and Technology
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    • 제55권3호
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    • pp.939-946
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    • 2023
  • Comprehensive Research Facility for Fusion Technology (CRAFT) is an integration of different demonstrating or testing facilities, which aim to develop the critical technology or composition system towards the fusion reactor. Due to the importance and challenge of the negative ion based neutral beam injection (NNBI), a NNBI test facility is included in the framework of CRAFT. The initial object of CRAFT NNBI test facility is to obtain a H0 beam power of 2 MW at the energy of 200-400 keV for the pulse duration of 100 s. Inside the negative ion accelerator of NNBI system, the interactions of the negative ions with the background gas and electrodes can generate abundant stray electrons. The stray electrons can be further accelerated and dumped on the electrodes or eject from the accelerator. The stray electrons, including the ejecting electrons, cause the unwanted particle and heat flux onto the electrodes and the inner components of beamline (especially the temperature sensitive cryopump). The suppression of the stray electrons from the CRAFT accelerator is carried out via a series of design and simulation works. The paper focuses the influence of different magnetic field configurations on the stray electrons and the character of the ejecting electrons.

기체크로마토그래프-질량분석기의 실리콘 분리막 인터페이스의 유용성 연구 (Feasibility study of membrane interface for gas chromatograph-mass spectrometry)

  • 강길선;이동수;이화심;박창준
    • 분석과학
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    • 제21권6호
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    • pp.495-501
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    • 2008
  • GC-MS 의 기존 인터페이스와 새로운 인터페이스의 차이점과 유용성을 판단하기 위하여 Agilent 5973 GC-MS의 capillary direct interface를 떼어내고 GC와 질량분석기 사이에 실리콘 membrane을 장착하여 membrane interface GC-MS의 분석 유용성을 조사하였다. 최대 $4.7m{\ell}/min$ 까지 헬륨 운반기체유량을 올릴 때 질량분석기의 진공도는 거의 영향을 받지 않으며, 피이크끌림 현상이 줄어들고 머무른시간이 줄어드는 빠른 분석을 보였다. Membrane 의 두께를 $127{\mu}m$에서 $75{\mu}m$으로 줄일 때 분리능이 향상 되며, membrane interface의 온도를 올릴 때 분리능과 감도가 향상되었다. 그러나 membrane interface GCMS는 질량/전하 비 73, 147에서 바탕이온이 발생하는 것과 기존의 capillary direct insertion interface보다 낮은 감도와 peak tailing에 의한 낮은 분리능의 문제점을 갖는다.

Ecophysiological characteristics of Rosa rugosa under different environmental factors

  • Young-Been Kim;Sung-Hwan Yim;Young-Seok Sim;Yeon-Sik Choo
    • Journal of Ecology and Environment
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    • 제47권3호
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    • pp.85-102
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    • 2023
  • Background: Ecophysiological characteristics of Rosa rugosa were analyzed under different environmental factors from May to October 2022. Photosynthesis, chlorophyll fluorescence, chlorophyll content, leaf water content (LWC), osmolality, carbohydrate content, and total ion content were measured to compare the physiological characteristics of R. rugosa at two study sites (i.e., in large pots and in the Goraebul coastal sand dune area). Results: When R. rugosa was exposed to high temperatures, photosynthetic parameters including net photosynthetic rate (PN) and stomatal conductance (gs) in both experiment areas declined. In addition, severe photoinhibition occurs when R. rugosa is continuously exposed to high photosynthetically active radiation (PAR), and because of this, relatively low Y(II) (i.e., the quantum yield of photochemical energy conversion in photosystem II [PSII]) and high Y(NO) (i.e., the quantum yield of non-regulated, non-photochemical energy loss in PSII) in the R. rugosa of the pot were observed. As the high Y(NPQ) (i.e., the quantum yield of regulated non-photochemical energy loss in PSII) of R. rugosa in the coastal sand dune, they dissipated the excessed photon energy through the non-photochemical quenching (NPQ) mechanism when they were exposed to relatively low PAR and low temperature. Rosa rugosa in the coastal sand dune has higher chlorophyll a and carotenoid content. The high chlorophyll a + b and low chlorophyll a/b ratios seemed to optimize light absorption in response to low PAR. High carotenoid content played an important role in NPQ. As a part of the osmotic regulation in response to low LWCs, R. rugosa exposed to high temperatures and continuously high PAR used soluble carbohydrates and ions to maintain high osmolality. Conclusions: We found that Fv/Fm was lower in the potted plants than in the coastal sand dune plants, indicating the vulnerability of R. rugosa to high temperatures and PAR levels. We expect that the suitable habitat range for R. rugosa will shrink and move to north under climate change conditions.

Methanol-involved heterogeneous transformation of ginsenoside Rb1 to rare ginsenosides using heteropolyacids embedded in mesoporous silica with HPLC-MS investigation

  • Mengya Zhao;Yusheng Xiao;Yanyan Chang;Lu Tian;Yujiang Zhou;Shuying Liu;Huanxi Zhao;Yang Xiu
    • Journal of Ginseng Research
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    • 제48권4호
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    • pp.366-372
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    • 2024
  • Background: The biological activity and pharmacological effects of rare ginsenosides have been proven to be superior to those of the major ginsenosides, but they are rarely found in ginseng. Methods: Ginsenoside Rb1 was chemically transformed with the involvement of methanol molecules by a synthesized heterogeneous catalyst 12-HPW@MeSi, which was obtained by the immobilization of 12-phosphotungstic acid on a mesoporous silica framework. High-performance liquid chromatography coupled with mass spectrometry was used to identify the transformation products. Results: A total of 18 transformation products were obtained and identified. Methanol was found to be involved in the formation of 8 products formed by the addition of methanol molecules to the C-24 (25), C-20 (21) or C-20 (22) double bonds of the aglycone. The transformation pathways of ginsenoside Rb1 involved deglycosylation, addition, elimination, cycloaddition, and epimerization reactions. These pathways could be elucidated in terms of the stability of the generated carbenium ion. In addition, 12-HPW@MeSi was able to maintain a 60.5% conversion rate of Rb1 after 5 cycles. Conclusion: Tandem and high-resolution mass spectrometry analysis allowed rapid and accurate identification of the transformation products through the characteristic fragment ions and neutral loss. Rare ginsenosides with methoxyl groups grafted at the C-25 and C-20 positions were obtained for the first time by chemical transformation using the composite catalyst 12-HPW@MeSi, which also enabled cyclic heterogeneous transformation and facile centrifugal separation of ginsenosides. This work provides an efficient and recyclable strategy for the preparation of rare ginsenosides with the involvement of organic molecules.

6가 크롬 처리를 위한 알루미늄 산화물을 함유한 재생 분말 폐기물의 적용 (Application of Reused Powdered Waste Containing Aluminum Oxide on the Treatment of Cr(VI))

  • 임재우;김태환;강형식;김도선;김한선;조석희;양재규;장윤영
    • 대한환경공학회지
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    • 제31권3호
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    • pp.179-185
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    • 2009
  • 본 연구에서는 알루미늄 산화물을 함유한 재생 분말 폐기물에 의한 Cr(VI)의 제거특성을 조사하였다. 가공하지 않은 폐기물의 유기물을 제거하기 위해 $550^{\circ}C$에서 소성하여 재생 분말 폐기물(RPW)을 준비하였다. 수용액 상에서 Cr(VI)의 흡착 경향에 관한 연구를 위해 회분식 반응장치를 이용하여 pH 변화, 흡착 속도, 등온 흡착 실험을 4가지 다른 이온세기 화학종($NO_3\;^-,\;CO_3\;^{2-},\;SO_4\;^{2-},\;PO_4\;^{3-}$)의 존재 하에서 수행하였다. $SO_4\;^{2-}$$PO_4\;^{3-}$가 존재할 때는 전체 pH 범위에서 크롬의 흡착이 크게 감소하였다. 반면 $NO_3\;^-$$CO_3\;^{2-}$에 의한 흡착 방해의 영향은 $SO_4\;^{2-}$$PO_4\;^{3-}$에 의한 것보다 상대적으로 낮았다. $NO_3\;^-$$CO_3\;^{2-}$의 존재 하에 Cr(VI) 흡착은 pH 4.5에서 최대로 나타났다. 이온세기 화학종의 농도가 증가함에 따라 Cr(VI)의 흡착은 감소하였다. 이러한 결과를 토대로 할때 RPW와 Cr(VI) 사이의 흡착은 외부배위권 착물을 통하여 발생되는 것으로 사료된다. RPW에 의한 Cr(VI)의 흡착은 2차 반응으로 잘 표현되었다. Langmuir 등온흡착식을 이용하여 pH 3에서 RPW에 의한 Cr(VI)의 최대 흡착량을 구한결과 $NO_3\;^-,\;CO_3\;^{2-},\;SO_4\;^{2-},\;PO_4\;^{3-}$가 이온세기 화학종으로 있을 때 각각 11.1, 10, 3.33, 5 mg/g으로 얻어졌다.