• 제목/요약/키워드: water+formic acid

검색결과 134건 처리시간 0.029초

Determination of Free Amino Acids in Isatidis Radix By HILIC-UPLC-MS/MS

  • Pan, Yilin;Li, Jin;Li, Xiang;Chen, Jianwei;Bai, Ganggang
    • Bulletin of the Korean Chemical Society
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    • 제35권1호
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    • pp.197-203
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    • 2014
  • A rapid, accurate and precise method for the determination of 22 amino acids in Isatidis Radix by Hydrophilic Interaction Ultra-High-Performance Liquid Chromatography Coupled with Triple-Quadrupole Mass Spectrometry (HILIC-UPLC-MS/MS) was established. Chromatographic separation was carried out on a Acquity UPLC BEH Amide column ($2.1mm{\times}100mm$, $1.7{\mu}m$) with gradient elution of acetonitrile (containing 0.05% formic acid and 2 mM ammonium formate) and water (containing 0.15% formic acid and 10 mM ammonium formate) at a flow rate of 0.4 mL/min; Waters Xevo$^{TM}$ TQ worked in multiple reaction monitoring mode. All components were separated in 17 min. All calibration curves were linear ($R^2$ > 0.991) over the tested ranges. The limits of detection (LOD) and limits of quantitation (LOQ) for these compounds were 0.21-79.55 and 0.72-294.23 ng/mL, respectively. The average recoveries were in the range of 93.75-104.16% with RSD value less than 6.56%. Therefore, this method could be an alternative assay for the determination of 22 amino acids in Isatidis Radix due to its rapidness, sensitivity, less sample and solvent consumption.

UPLC를 이용한 지역별 헛개나무(Hovenia dulcis) 플라보노이드의 정량분석 (Quantitative Analys is of Flavonoids in Hovenia dulcis by Region Using UPLC)

  • 이동환;김현준
    • 한국자원식물학회:학술대회논문집
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    • 한국자원식물학회 2022년도 추계학술대회
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    • pp.100-100
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    • 2022
  • Hovenia dulcis is a herbal plant, which belongs to the Rhamnaceae family and is a native of Japan, China and Korea. Its fruit stalk is called 'Jiguja' in Korea. It has been traditionally used as a medicinal plant in East Asia. It was reported to have detoxification effects on alcohol poisoning, and antioxidant, antidiabetic etc. Sample of 5 g was extracted with 50 mL of 70% EtOH. The supernatant was filtered by 0.45 ㎛ membrane filter before analysis. The UPLC system was performed on Waters alliance UPLC HSS T3 column (2.1 × 100 mm, 1.7 ㎛) with a UV detector. The gradient system was a binary eluent of 0.1% formic acid in water(A) and 0.1% formic acid in acetonitrile(B) with gradient conditions as follows: Initial, 10% B; 1 min, 10% B; 4 min, 20% B; 10 min, 25% B; 12 min, 30% B; 14 min, 90% B; 17 min, 90% B; flow rate of 0.2 mL/min. The samples were injected by 2 µL and were detected at UV 355 nm. As a result of analysis, chromatographic patterns appeared in two cases: samples analyzed for ampelopsin and myricetin, and samples analyzed for taxifolin and quercetin. Among the four compounds, the largest regional difference was found to be taxifolin.

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주요 사료작물의 곤포 Silage 조제이용에 관한 연구 II. 생육단계별 건물축적형태화 곤포사일리지 조제이용 (Study on Baled Silage Making of Selected Forage Crop and Pesture Grasses II. Yield performance and nutritieve evaluation of baled silage as affected by stage of growth)

  • 김정갑;한민수;김건엽;한정대;강우성;신정남
    • 한국초지조사료학회지
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    • 제15권3호
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    • pp.198-206
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    • 1995
  • 본 연구는 1991년부터 1993년까지 사료작물과 목초류 7종(호맥, 대맥, 연맥, Italian ryegrass, alfalfa, orchardgrass 및 혼과목초)을 공시재료로 하여 곤포사일리지(BS=baled silage making)조제이용을 위한 수확시기와 이때의 BS 생산성 및 품질을 평가하였다. 시험방법에 있어서 작물재배는 농촌진흥청의 사료작물 및 목초 표준경종방법에 준하여 실시하였다. 사일리지 조제작업중 BS는 자체적으로 제작한 각형 베일러를 이용 개체당 크기 90cm$\times$60cm$\times$50cm, 중량은 건물기준 20kg 내외, 곤포압착 21~23mm를 유지하여 조제하였다. 한편 고수분 재료는 수분정도에 따라 예건처리(무처리, 0.5일 및 1.0일)와 formic acid(무처리, 0.3% 및 0.6%)를 병행 처리하여 BS 를 조제하였다. 맨류작물의 BS 생산을 위한 수확적기는 대맥, 황숙기, 호맥과 연맥은 유숙기 이었으며 이때의 BS 수량은 각각 11.92톤(대맥), 12.64톤(호맥) 및 8.41톤/ha(연맥)이었다. Italian ryegrass 및 목초의 수확적기는 각 초종 모두 개화기로서 년간 BS 생산성은 Italian 13.81톤(2회 예취), 혼파목초 11.46톤(3회), alfalfa 10.62톤/ha(3회)이었다. 한편 조기수확에 따른 고수분 재료의 BS 품질은 무처리시의 35점에서 예건 및 FA 동시처리시에는 84점으로 향상되었다. Italian tyegrass의 BS품질도 무처리시의 61점에서 예건 및 FA 처리시에는 88점으로 개선되는 효과가 있었다.

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Effect of heat treatment on the structural characteristics and properties of silk sericin film

  • Park, Chun Jin;Um, In Chul
    • International Journal of Industrial Entomology and Biomaterials
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    • 제37권2호
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    • pp.36-42
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    • 2018
  • Recently, silk sericin has attracted attention because of its unique properties as a biomaterial, including its UV resistance, moisturizing effect on skin, and wound-healing effect. Therefore, the preparation of sericin in various forms such as gel, film, fiber, and sponge is studied for cosmetic and biomedical applications, and the effect of the preparation conditions on the structure and properties of sericin forms is examined to maximize its performance. In this study, silk sericin films were prepared under different preparation conditions and heat-treated at high temperatures ($100-250^{\circ}C$) to examine the effect of heat treatment on the film structure. The order of the crystallinity index of the untreated sericin film is as follows: F25 (sericin film cast from formic acid) > WE25 (ethanol treated sericin film cast from water at $250^{\circ}C$) > W25 (sericin film cast from water at $250^{\circ}C$) > W100 (sericin film cast from water at $100^{\circ}C$). As the heat-treatment temperature was increased, the color of the sericin films changed gradually from colorless to yellow, brown, and black depending on the temperature. The crystallinity of the sericin film changed after the heat treatment, depending on the preparation condition. Whereas a sericin film cast from formic acid (F25) started to lose its crystallinity at $200^{\circ}C$, thus undergoing the highest loss of crystallinity among the sericin films studied, the rest (W25, WE25, and W100) showed a decrease in crystallinity at $250^{\circ}C$, owing to the disruption of the ${\beta}$-sheet crystallites due to heat.

수소생산균 Enterobacter cloacae YJ -1의 분리 및 특성 (Isolation and Characterization of Hydrogen Producing Bacterium)

  • 이기석;강창민;정선용
    • KSBB Journal
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    • 제18권2호
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    • pp.149-154
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    • 2003
  • 수소를 생산하기 위하여 자연계로부터 분리된 균주는 Enterebacter cloacae로 동정되었으며 이 균주를 YJ-1으로 명명하였다. 수소발생량을 기준하여 이 균주의 최적 성장조건을 살펴본 바, 회분식 배양에서 $35^{\circ}C$, pH 7.5로 나타났다. 따라서 탄소원의 농도를 변화시킨 결과, 최대의 수소생산은 2% glucose, 4% sucrose, 5% fructose에서 각각 950 mL/L, 1000 mL/L, 948 mL/L을 얻어졌으며, 초기에 비해 2.5배 높은 생산량을 얻을 수 있었다. 유기산 축척에 따른 pH 저하를 막기 위해 완충제인 phosphate를 첨가한 결과, 50 mM에서 가장 높은 수소를 생산할 수 있었다. 반회분식 배양으로 50%의 새로운 배지를 8 hr 간격으로 치환하여 48시간동안 수행한 결과 1920 mL/L의 수소를 생산할 수 있었다. Yeast extract는 균체성장에 중요한 성분으로서 0.5%에서 최대의 수소를 생산할 수 있었다. 발효 중 생성된 유기산은 대부분 formic acid, acetic acid이고 적은 양의 propionic acid가 생성되었다.

Marker compounds contents of Salvia miltiorrhiza Radix depending on the cultivation regions

  • Seong, Gi-Un;Kim, Mi-Yeon;Chung, Shin-Kyo
    • Journal of Applied Biological Chemistry
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    • 제62권2호
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    • pp.129-135
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    • 2019
  • Salvia miltiorrhiza Radix is cultivated in Korea and China and is traditionally used to treat cardiovascular diseases. In this study, we developed and validated a quantitative analysis method for S. miltiorrhiza Radix using high-performance liquid chromatography (HPLC). Identification was performed using ultra performance liquid chromatography-tandem mass spectrometry. For quantitative analysis, we used seven marker compounds. Separation conditions for HPLC were optimized using an ODS column with gradient conditions of 1% formic acid in distilled water and 1% formic acid in acetonitrile, with a flow rate of 0.8 mL/min and a detection wavelength of 280 nm. This method showed good linearity ($R^2=0.9998$), precision (relative standard deviation ${\leq}3.3%$), accuracy (recovery of 94.16-102.89%), limit of detection ($7.53{\mu}g/mL$), and limit of quantification ($23.71{\mu}g/mL$). This approach successfully quantified marker compounds in S. miltiorrhiza Radix. The individual marker compounds were identified by comparing the molecular masses and retention times with does standard compounds. Marker compound contents of S. miltiorrhiza Radix were investigated with different cultivation regions. Seven marker compounds were detected and quantified in all samples. Among them, salvianolic acid B showed the highest contents and it ranged from 4.13 to 7.15%. The salvianolic acid B content (7.15%) of marker compound was the highest in Bonghwa, and the tanshinone IIA content (1.90%) was the highest in Pohang. The results of marker compounds and developed method were intended to provide a favorable reference for the study of S. miltiorrhiza Radix from different regions of Korea.

$\etha$-N-[(2-Chloroethyl) nitrosocarbamoyl]-L-lysine의 합성 (Preparation of $\etha$-N-[(2-Chloroethyl) nitrosocarbamoyl]-L-lysine)

  • 김정균;조인섭
    • 약학회지
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    • 제27권2호
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    • pp.177-179
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    • 1983
  • A copper complex of $\epsilon$-N-[(2-chloroethyl)carbamoyl]-L-lysine was prepared by the treatment of the L-lysine copper complex with 2-chloroethyl isocyanate in cold water. Within the L-lysine copper complex molecule, the $\alpha-amino$ and carboxyl groups are bounded to $Cu^{2+}$ but the $\epsilon-amino$ group is free and can react with carbamoylating agents. A potential antitumor agent, $\epsilon-N-[(2-chloroethyl)$ nitrosocarbamoyl]-L-lysine was synthesized by nitrosation of this copper complex with Na $NO_{2}$ in anhydrous formic acid, followed by the passage of $H_{2}$S gas.

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뽕잎(桑葉)에 함유된 항산화성 물질 (Antioxidative Substances in Mulberry Leaves)

  • 신두호
    • 한국응용과학기술학회지
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    • 제15권3호
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    • pp.27-31
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    • 1998
  • Antioxodative substances in Mulberry leaves were examined. Antioxidative substances in Mulberry leaves were extracted by 80% methanol agueous solution. Antioxidative activity of extract was determined by examining hydrogen donating ability on 1,1-diphenyl-2-picrylhydrazyl (DPPH) and the inhibitory effect on the formation of the peroxide from Linoleic acid in the test tube at $50^{\circ}C$. Antioxidative substance were, then, separated and indentified by thin layer chromatography(TLC), UV-Vis spectrum and High performance liquid chromatography(HPLC) methods. Hydrogen donating ability on DPPH and antioxidative ability on linoleic acid of the extracted antioxidative substance were higher than those of 100ppm butylated hydroxy toluene(BHT). The extracted antioxidative substances were separated by TLC using ethylacetate : chloroform : formic acid : water(8 : 1 : 1 : 1 v/v) as a solvent, and a spot at Rf=0.35 was detected. The spot was scraped from the plate, and extrated by methanol. The extract was analyzed by UV-Vis spetra and HPLC, and chlorogenic acid was identified as a antioxidative substance.

TLC 이용한 젖산 분리와 정량분석 개발을 위한 연구

  • 조갑수;최미화;류화원;김근아;유선균;김도만
    • 한국생물공학회:학술대회논문집
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    • 한국생물공학회 2002년도 생물공학의 동향 (X)
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    • pp.165-168
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    • 2002
  • TLC(Thin Layer Chromatography) 는 제약산업이나 생화학 연구 그리고 여러 산업 현장에서 널리 이용되는 화학 분석 방법이다 . 본 연구에서는 적은 비용으로도 많은 양의 시료를 신속하게 분리할 수 있는 TLC를 이용하여 유기산인 젖산 (Lactic acid) 을 분리는 전개방법을 개발하였다 . 전개용매는 2 가지 용매 (1) nitroethane nitromethane : ethanol: water: I-propanol = 1 : 2 : 3 : 4 : 5 (v/v/v/v/v), (2) diisopropyl ether. formic acid. water = 90 : 7 : 3 (v/v/v) 를 사용하였다 . 발색시약은 A : bromocresol purple reagent I, B . bromocresol purple reagent II, C : bromocresol green-bromophenol blue-potassium permanganate reagent 를 사용하여 분석하는 방법을 개발하였다 $^6)$. 젖산의 분리는 silica gel TLC plate를 이용하는 경우 , 용매 (1) 에 발색시약 B를 사용했을 때 , 분리 확인이 가장 좋았다.

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구실잣밤나무 열매의 성분분석 및 항산화활성 평가 (Component Analysis and Antioxidative Activity of Castanopsis cuspidata var. sieboldii Nut)

  • 이승제;안기완;최태수;정형석;문제학;박근형
    • 한국식품저장유통학회지
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    • 제17권1호
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    • pp.139-144
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    • 2010
  • 난대성 상록활엽수종의 자원화 및 식품 소재화 탐색을 목적으로 구실잣밤나무(Castanopsis cuspidata var. sieboldii $N_{AKAI}$) 열매(구실잣밤) 추출물의 수율, pH, 당도, 색도, 구성당, 유기산 함량, 페놀 함량 및 항산화활성을 검정하였다. 각 용매에 대한 추출물의 수율은 물 추출물에서 3.6%로 가장 높았고, pH는 6.43의 중성값을 보였으며, 당도는 3.17 $^{\circ}Brix$를 나타내었다. 색도 중 L값은 83.07, a값은 1.49 그리고 b값은 10.48을 나타내었다. 구성당의 조성 및 함량은 fructose 27.11 mg%, glucose 26.29 mg%, galactose 0.86 mg%로 나타났다. 유기산은 총 5종이 동정되었으며, oxalic acid(59.44%), formic acid (23.99%), malic acid (11.24%), citric acid (3.34%), succinic acid (1.99%) 순으로 나타났다. 총 페놀 함량은 물 추출물에서 27.69 mg% 수준으로 가장 높았고, DPPH radical-scavenging 활성은 대조구인 $\alpha$-tocopherol ($SC_{50}\;12.47{\mu}g/mL$)에 비해 낮은 수준이었으나 EtOAc 추출물($SC_{50}\;74.88{\mu}g/mL$)에서 가장 강한 활성을 보였다. 이와 같은 결과를 바탕으로 구실잣밤은 다양한 식품소재 및 기능성 소재로서의 활용성이 기대되었으며, 또 도토리의 대용 및 병용이 가능한 소재로서 실용화 가능성이 확인되었다.