• 제목/요약/키워드: Formic Acid

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감마선 조사에 의한 hexahydro-1,3,5-trinitro-1,3,5-triazine(RDX)의 분해 (Decomposition of Hexahydro-1,3,5-trinitro-1,3,5-triazine by Gamma Ray Irradiation)

  • 이병진;이면주;김유리
    • 상하수도학회지
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    • 제18권6호
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    • pp.731-741
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    • 2004
  • The purpose of this study was to evaluate the potential of a gamma ray irradiation to decompose hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) in an aqueous solution. The decomposition reaction of RDX by gamma ray irradiation was a first-order kinetic over the applied initial concentrations (10-40mg/L). The dose constant was strongly dependent on the initial concentration of the RDX. The removal of RDX was more efficient at pH below 3 and at pH above 11 than at neutral pH (pH 5-9). The required irradiation dose to remove 99% of the RDX (40mg/L) was 4, 8 and 1 kGy, at pH 2, 7 and 13, respectively. The dose constant was increased by two folds and over twelve folds at pH 2 and 13, respectively, when compared with that at pH 7. When an irradiation dose of 20 kGy was applied, the removal efficiencies of TOC were 80, 57 and 91% at pH 2, 7 and 13, respectively. Ammonia and nitrate were detected as the main nitrogen byproducts of RDX and formic acid was detected as an organic byproduct. The results showed that a gamma ray irradiation was an attractive method for the decomposition of RDX in an aqueous solution and it was found that a strong alkaline pH over 12 should be applied to the decomposition reaction of RDX.

친환경용매 기반의 술폰화 폴리아릴렌 에테르 술폰 랜덤 공중합체 Thin Film Composite 제조 (Preparation of Disulfonated Poly(arylene ether sulfone) Random Copolymer Thin Film Composite Membranes Using a Benign Solvent)

  • 이창현;제임스 맥그라스;베니프리만
    • 멤브레인
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    • 제24권4호
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    • pp.292-300
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    • 2014
  • 내염소성을 갖는 염제거공정용 술폰화 폴리아릴렌 에테르 술폰 랜덤 공중합체(SPAES) thin film composite (TFC)막이 모노글라임 용매를 이용하여 제조되었다. 모노글라임은 선택층인 SPAES만을 용해시키며, 다공성 폴리술폰(예 : Udel$^{(R)}$)층에 대해 비용해성을 지녀, TFC 제조를 위한 선택적 용매로 사용될 수 있다. 또한 개미산이나 디에틸글리콜과는 달리, 환경적으로 무해하며, 매우 낮은 끊는점을 지녔다는 점이 또 다른 장점이 될 수 있다. 다공성 Udel$^{(R)}$ 지지체 위에 코팅시, 코팅용액이 기공구조에 침투하여 유수량을 감소시키는 기공투과현상이 발생하는데, 이를 최소화하기 위해 지지체를 이소프로필알콜과 글리세린 혼합액에서 전처리 후에, 코팅-건조 공정을 통해 결함이 없는 SPAES TFC로 제조된다. 또한, SPAES 선택층의 술폰화도, 고정이온의 염상태 및 물리-화학적 가교효과를 SPAES TFC막을 통한 투과거동과 관련하여 관찰하였다.

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

  • 신상은;조현우;명승운
    • 분석과학
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    • 제23권4호
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    • pp.405-413
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    • 2010
  • 축산물(소의 근육 및 간)중에 잔류하는 합성 글루코코티코이드 6종 (betamethasone, dexamethasone, prednisone, prednisolone, methylprednisolone, flumethasone)에 대한 동시분석방법을 확립하였다. 효과적인 기기분석을 위해서 시료는 C18 고체상 카트리지를 사용하여 에틸아세테이트 용매를 사용하여 추출/정제하였다. C18 컬럼을 사용하여 분리한 후 음이온 전기분무 질량분석법의 multiple reaction monitoring 방법을 사용하여 정량 및 정성 분석을 수행하였다. 효과적이고 감도있는 HPLC-MS/MS 분석을 위해서 0.1% 포름산이 포함된 물과 아세토나이트릴이 이동상 용매로 사용되었다. 메트릭스와 약물의 종류에 따라서 검출한계(LOD)는 $0.2-0.1\;{\mu}g$/kg, 정량한계(LOQ)는 $0.8-3.4{\mu}g$/kg 이었으며, 회수율은 89.5-119.6%이었다. 확립된 기존의 방법들에 비해 6종의 글루코코티코이드의 동시분석 방법이 간소화되었고, 좋은 정확도, 정밀도 및 회수율을 나타내었으며, 축산 육류 중에 잔류하는 글루코코티코이드들 분석하는데 사용될 수 있을 것이다.

Qualitative Analysis of the Major Constituents in Traditional Oriental Prescription Bang-poong-tong-sung-san by Liquid Chromatography/Ultraviolet Detector/Ion-Trap Time-of-Flight Mass Spectrometry

  • Eom, Han Young;Kim, Hyung-Seung;Han, Sang Beom
    • Mass Spectrometry Letters
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    • 제5권1호
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    • pp.24-29
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    • 2014
  • An advanced and reliable high performance liquid chromatography (HPLC)/ultraviolet detector (UV)/ion-trap time-of-flight (IT-TOF) mass spectrometry was developed for the simultaneous quantification of 19 marker compounds in Bang-poong-tong-sung-san (BPTS), a traditional oriental prescription. Various parameters affecting HPLC separation and IT-TOF detection were investigated, and optimized conditions were identified. The separation was achieved on a Capcell PAK C18 column ($1.5mm{\times}250mm$, $5{\mu}m$ particle size) using a gradient elution of acetonitrile and water containing 0.1% formic acid at a flow rate of 0.1 mL/min. The column temperature was maintained at $40^{\circ}C$ and the injection volume was $2{\mu}L$. IT-TOF system was equipped with an electrospray ion source (ESI) operating in positive or negative ion mode. The optimized electrospray ionization parameters were as follows: ion spray voltage, +4.5 kV (positive ion mode), or -3.5 kV (negative ion mode); drying gas ($N_2$), 1.5 L/min; heat block temperature, $200^{\circ}C$. Automatic $MS^n$ (n = 1~3) analyses were carried out to obtain structural information of analytes. Elemental compositions and their mass errors were calculated based on their accurate masses obtained from a formula predictor software. The marker compounds in BPTS were identified by comparisons between $MS^n$ spectra from standards and those from extracts. Moreover, the libraries of $MS^2$ and $MS^3$ spectra and accurate masses of parent and fragment ions for marker compounds were constructed. The developed method was successfully applied to the BPTS extracts and identified 17 out of 19 marker compounds in the BPTS extracts.

Comparison of Anthocyanin Content in Seed Coats of Black Soybean [Glycine max(L.) Merr.] Cultivars Using Liquid Chromatography Coupled to Tandem Mass Spectrometry

  • Shin, Sung-Chul;Lee, Soo-Jung;Lee, Sung-Joong;Chung, Jong-Il;Bae, Dong-Won;Kim, Soo-Taek;Sung, Nak-Ju
    • Food Science and Biotechnology
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    • 제18권6호
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    • pp.1470-1475
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    • 2009
  • The seed coat of the black soybean contains 3 main anthocyanins such as delphinidin-3-O-$\beta$-glucoside, cyanidin-3-O-$\beta$-glucoside, and petunidin-3-O-$\beta$-glucoside. As a part of our effort on discovering and breeding new black soybean cultivars which possesses specific anthocyanin component rich, we determined the anthocyanin profiles of the 2 cultivars recently developed soybean cv. Gaechuck #1 and cv. Gyeongsang #1, using liquid chromatography-tandem mass spectrometry (LC-MS/MS) and compared their content and identity with those of previously known 10 cultivar controls. The Cosmosil-$5C_{18}$-AR-II column were selected for the analysis because of the best peak separation. The column temperature was set up at $35^{\circ}C$. The mobile phase consisting of water containing 0.5%(v/v) formic acid and methanol gave good separation between the 3 anthocyanin analytes and internal standard (quercetin 3-O-$\beta$-rutinoside) and peaks with suppressed tail. The MS/MS spectra of each individual anthocyanin standard were detected in positive electron spray ionization (ESI) modes. It was disclosed that the anthocyanin contents of the soybean cv. Gaechuck#1 and cv. Gyeongsang#1 are roughly higher than those of the 10 controls.

High-temperature Adhesion Promoter Based on (3-Glycidoxypropyl) Trimethoxysilane for Cu Paste

  • Jiang, Jianwei;Koo, Yong Hwan;Kim, Hye Won;Park, Ji Hyun;Kang, Hyun Suk;Lee, Byung Cheol;Kim, Sang-Ho;Song, Hee-Eun;Piao, Longhai
    • Bulletin of the Korean Chemical Society
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    • 제35권10호
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    • pp.3025-3029
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    • 2014
  • To realize copper-based electrode materials for printed electronics applications, it is necessary to improve the adhesion strength between conductive lines and the substrate. Here, we report the preparation of Cu pastes using (3-glycidoxypropyl) trimethoxysilane (GPTMS) prepolymer as an adhesion promoter (AP). The Cu pastes were screen-printed on glass and polyimide (PI) substrates and sintered at high temperatures (> $250^{\circ}C$) under a formic acid/$N_2$ environment. According to the adhesion strengths and electrical conductivities of the sintered Cu films, the optimized Cu paste was composed of 1.0 wt % GPTMS prepolymer, 83.6 wt % Cu powder and 15.4 wt % vehicle. After sintering at $400^{\circ}C$ on a glass substrate and $275^{\circ}C$ on a PI substrate, the Cu films showed the sheet resistances of $10.0m{\Omega}/sq$. and $5.2m{\Omega}/sq$., respectively. Furthermore, the sintered Cu films exhibit excellent adhesion properties according to the results of the ASTM-D3359 standard test.

Determination of Non-Steroidal Anti-Inflammatory Drugs in Human Urine Sample using HPLC/UV and Three Phase Hollow Fiber-Liquid Phase Microextraction (HF-LPME)

  • Cha, Yong Byoung;Myung, Seung-Woon
    • Bulletin of the Korean Chemical Society
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    • 제34권11호
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    • pp.3444-3450
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    • 2013
  • Three phase hollow fiber-liquid phase microextraction (HF-LPME), which is faster, simpler and uses a more environmentally friendly sample-preparation technique, was developed for the analysis of Non-Steroidal Anti-Inflammatory Drugs (NSAIDs) in human urine. For the effective simultaneous extraction/concentration of NSAIDs by three phase HF-LPME, parameters (such as extraction organic solvent, pH of donor/acceptor phase, stirring speed, salting-out effect, sample temperature, and extraction time) which influence the extraction efficiency were optimized. NSAIDs were extracted and concentrated from 4 mL of aqueous solution at pH 3 (donor phase) into dihexyl ether immobilized in the wall pores of a porous hollow fiber, and then extracted into the acceptor phase at pH 13 located in the lumen of the hollow fiber. After the extraction, 5 ${\mu}L$ of the acceptor phase was directly injected into the HPLC/UV system. Simultaneous chromatographic separation of seven NSAIDs was achieved on an Eclipse XDB-C18 (4.6 mm i.d. ${\times}$ 150 mm length, 5 ${\mu}m$ particle size) column using isocratic elution with 0.1% formic acid and methanol (30:70) at a HPLC-UV/Vis system. Under optimized conditions (extraction solvent, dihexyl ether; $pH_{donor}$, 3; $pH_{acceptor}$, 13; stirring speed, 1500 rpm; NaCl salt, 10%; sample temperature, $60^{\circ}C$; and extraction time, 45 min), enrichment factors (EF) were between 59 and 260. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of 5-15 ng/mL and 15-45 ng/mL, respectively. The relative recovery and precision obtained were between 58 and 136% and below 15.7% RSD, respectively. The calibration curve was linear within the range of 0.015-0.96 ng/mL with the square of the correlation coefficient being more than 0.997. The established method can be used to analyse of NSAIDs of low concentration (ng/mL) in urine.

Pentafluorophenylprophyl Ligand-based Liquid Chromatography-Tandem Mass Spectrometric Method for Rapid and Reproducible Determination of Metformin in Human Plasma

  • Yang, Jeong Soo;Oh, Hyeon Ju;Jung, Jin Ah;Kim, Jung-Ryul;Kim, Tae-Eun;Ko, Jae-Wook;Lee, Soo-Youn;Huh, Wooseong
    • Bulletin of the Korean Chemical Society
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    • 제34권11호
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    • pp.3284-3288
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    • 2013
  • This paper describes first development and validation of pentafluorophenylprophyl ligand-based liquid chromatography coupled to tandem mass spectrometry (PFPLC-MS/MS) method to determine metformin, a highly polar compound, in human plasma. Metformin and Phenformin (internal standard) were extracted from human plasma 50 ${\mu}L$ with a single-step protein precipitation. The chromatographic separation was performed using a linear gradient elution of mobile phase involving 5.0 mM ammonium formate solution with 0.1% formic acid (A) and acetonitrile (B) over 3.0 min of run time on a Phenomenex Luna PFP column. The detection was performed using a triple-quadrupole tandem mass spectrometer (Waters Quattro micro) with electrospray ionization in the mode of positive ionization and multiple-reaction monitoring (MRM). The developed method was validated with 5.0 ng/mL of lower limit of quantification (LLOQ). The calibration curve was linear over 5-3000 ng/mL of the concentration range ($R^2$ > 0.99). The specificity, selectivity, carry-over effect, precision, accuracy and stability of the method met the acceptance criteria. The method developed in this study had had rapidness, simplicity and ruggedness. The reliable method was successfully applied to high throughput analysis of real samples for a practical purpose of a pharmacokinetic study.

Rapid separation and identification of 31 major saponins in Shizhu ginseng by ultra-high performance liquid chromatography-electron spray ionization-MS/MS

  • Sun, Ting-Ting;Liang, Xin-Lei;Zhu, He-Yun;Peng, Xu-Ling;Guo, Xing-Jie;Zhao, Long-Shan
    • Journal of Ginseng Research
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    • 제40권3호
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    • pp.220-228
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    • 2016
  • Background: Among the various ginseng strains, Shizhu ginseng is endemic to China, mainly distributed in Kuandian Manchu Autonomous County (Liaoning Province, China); however, not much is known about the compounds (especially saponins) in Shizhu ginseng. Methods: A rapid, sensitive, and reliable ultra-high performance liquid chromatography coupled with MS/MS (UHPLC-MS/MS) method was developed to separate and identify saponins in Shizhu ginseng. Results: The separation was carried out on a Waters ACQUITY UPLC BEH $C_{18}$ column ($100mm{\times}2.1mm$, $1.7{\mu}m$) with acetonitrile and 0.1% formic acid aqueous solution as the mobile phase under a gradient elution at $40^{\circ}C$. The detection was performed on a Micromass Quattro Micro API mass spectrometer equipped with electrospray ionization source in both positive and negative modes. Under the optimized conditions, a total of 31 saponins were identified or tentatively characterized by comparing retention time and MS data with related literatures and reference substances. Conclusion: The developed UHPLC-MS/MS method was suitable for identifying and characterizing the chemical constituents in Shizhu ginseng, which provided a helpful chemical basis for further research on Shizhu ginseng.

Antibacterial activity of supernatant obtained from Weissella koreensis and Lactobacillus sakei on the growth of pathogenic bacteria

  • Im, Hana;Moon, Joon-Kwan;Kim, Woan-Sub
    • 농업과학연구
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    • 제43권3호
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    • pp.415-423
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    • 2016
  • This study was carried out to obtain basic data for the industrial use of Weissella koreensis and Lactobacillus sakei. The antibacterial activity of supernatants obtained from W. koreensis and L. sakei were tested against pathogenic bacteria such as Escherichia coli KCCM 11234, Salmonella enteritidis KCCM 3313, Salmonella enteritidis KCCM 12021, Salmonella typhimurium KCCM 40253, and Salmonella typhimurium KCCM 15. The supernatant of L. sakei showed antibacterial activity against E. coli KCCM 11234, S. enteritidis KCCM 12021, and S. typhimurium KCCM 15, while the supernatant of W. koreensis showed antibacterial activity against E. coli KCCM 11234 and S. enteritidis KCCM 12021. The effect of pH changes and heat treatment on antibacterial activity of the supernatants was examined using the sensitive pathogenic bacteria (E. coli KCCM 11234, S. enteritidis KCCM 12021 and S. typhimurium KCCM 15). Antibacterial activity against sensitive pathogenic bacteria was maintained under heat treatment at all temperatures, but there was no antibacterial activity associated with pH modification. Furthermore, it was confirmed that the antibacterial activity of the supernatants obtained from W. koreensis and L. sakei was a result of organic acids including, lactic, acetic, phosphoric, succinic, pyroglutamic, citric, malic, and formic acids. Therefore, the present study showed that the organic acids produced by L. sakei and W. koreensis exhibited a strong antibacterial activity against pathogenic bacteria. Moreover, in the food industry, these organic acids have the potential to inhibit the growth of pathogenic bacteria and improve the quality of stored food.