• Title/Summary/Keyword: Ammonium Acetate

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Synthesis, Docking Study and In-vitro Evaluation of Anti-Tuberculosis Activity of Tri Substituted Imidazoles Containing Quinoline Moiety

  • Sahana, S.;Vijayakumar, G.R.;Sivakumar, R.;Sriram, D.;Saiprasad, D.V.
    • Journal of the Korean Chemical Society
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    • v.66 no.3
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    • pp.194-201
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    • 2022
  • A simple, efficient, and cost-effective method has been employed for the synthesis of 2,4,5-trisubstituted imidazole derivatives (3a-j) containing quinoline substituent at 2nd position. Title compounds were obtained by multicomponent reaction (MCR), involving aryl substituted 1,2-diketone, quinoline carbaldehyde and ammonium acetate in the presence of acetic acid solvent under mild reaction conditions. The newly synthesized quinoline containing imidazole derivatives were confirmed through FT-IR, 1H-NMR, 13C-NMR and mass spectral analysis. In-vitro microplate alamar blue assay (MABA) to determine the MIC (minimum inhibitory concentration) values against Mycobacterium tuberculosis H37Rv was performed for the synthesized compounds. The synthesized compounds exhibited activity against Mycobacterium tuberculosis and among which compounds, 3d, 3f and 3i showed good activity. The highest activity was showed with compound 3i. The anti-mycobacterial activity results are well correlated with the computational molecular docking analysis, which was performed for the synthesized compounds prior to the evaluation of the activity.

Validation and measurement uncertainty of HPLC method for simultaneous determination of 10 dyes in adulterated Phellodendron

  • Lim, Suji;Yun, Choong-In;Ko, Kyung Yuk;Kim, Young-Jun
    • Korean Journal of Food Science and Technology
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    • v.53 no.4
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    • pp.391-398
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    • 2021
  • As global interest in herbal medicines has increased, the adulteration of herbal medicines has become a critical safety issue. Adulteration with dyes to improve the appearance of low-quality products is of particular concern. This study aimed to develop a high-performance liquid chromatography (HPLC) method to detect dyes added as adulterants to Phellodendron. Samples were analyzed on a C18 column using 50 mM ammonium acetate and acetonitrile as the mobile phase. All calibration curves showed good linearity (r2 ≥0.9999) over the five-point concentration range (1-50 mg/kg). Limit of detection ranged from 0.04-0.35 mg/kg, and limit of quantification ranged from 0.11-1.07 mg/kg. The repeatability and reproducibility for these measurements were 94.2-103.3% and 96.6-103.8% for accuracy and 0.14-2.28 RSD (%) and 0.80-2.37 RSD (%) for precision. Moreover, the measurement uncertainty of the low, medium, and high concentrations for 10 dyes was considered. Thus, this HPLC method is suitable for detecting color adulteration of Phellodendron.

Influence of Medium Composition on the Production of $\gamma$-Linolenic Acid by Mucor sp. KCTC 8405P (Mucor sp. KCTC 8405P의 배지조성이 감마 리놀렌산의 생산에 미치는 영향)

  • Kang, Hun-Seung;Shin, Hyun-Kyung
    • Microbiology and Biotechnology Letters
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    • v.17 no.6
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    • pp.568-573
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    • 1989
  • As a way to determine the optimal culture conditions for the production of ${\gamma}$-linolenic acid by Mucor sp. KCTC 8405P, the influence of different carbon and nitrogen sources, initial pH, and C/N ratio of medium was investigated. Glucose was found to be the best carbon source in terms of lipid content and ${\gamma}$-linolenic acid yield. Ammonium sulfate and organic nitrogen sources such as urea and peptone resulted in relatively increased lipid and ${\gamma}$-linolenic acid production. The highest accumulation of lipid was obtained at a C/N ratio of 56.6 using glucose and (NH$_4$)$_2$SO$_4$ as carbon and nitrogen source, respectively. It was found that the lipid content increased significantly with increasing initial pH of medium up to pH 9.0. The influence of mixed carbon source on the ${\gamma}$-linolenic acid yield was also investigated. High accumulation of lipids, 315 mg/100 ml medium, and 13-14% of ${\gamma}$-linolenic acid content in the cellular lipid were obtained in a shaking culture containing 3% of glucose and 2% sodium acetate as carbon source and 0.1% of (NH$_4$)$_2$SO$_4$ as nitrogen source at pH 8.0.

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Validation of LC-MS/MS Method for Determination of Rabeprazole in Human Plasma : Application of Pharmacokinetics Study (인체 혈장중 라베프라졸의 정량을 위한 LC-MS/MS 분석법 검증 및 단일 용량 투여에 의한 약물동태 연구)

  • Tak, Sung-Kwon;Seo, Ji-Hyung;Ryu, Ju-Hee;Choi, Sang-Joon;Lee, Myung-Jae;Kang, Jong-Min;Lee, Jin-Sung;Hong, Seung-Jae;Yim, Sung-Vin;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
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    • v.39 no.1
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    • pp.73-78
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    • 2009
  • A simple LC-MS/MS method of rabeprazole in human plasma was developed and validated. Rabeprazole and Internal standard (I.S), omeprazole, were extracted from human plasma by liquid liquid extraction, chromatographic separation of rabaprazole in plasma was achieved at $45^{\circ}C$ with a Shiseido UG120 $C_{18}$ column and methanol-10 mM ammonium acetate buffer (pH 9.42 with ammonium water), as mobile phase. Rabeprazole produced a protonated precursor ion [$(M+H)^+$] at m/z 360.10 and corresponding product ion at m/z 242.21. Internal standard produced a protonated precursor ion [$(M+H)^+$] at 346.09 and corresponding product ion at m/z 198.09. This method showed linear response over the concentration range of $1{\sim}500\;ng/mL$ with correalation coefficient greater than 0.99. The lower limit of quantitation (LLOQ) using 0.2 mL plasma was 1 ng/mL, which was sensitive enough for pharmacokinetics studies. The method was specific and validated with a limit of quantitation of 1 ng/mL. The intra-day and inter-day precision and accuracy were acceptable for all samples including the LLOQ. The applicability of the method was demonstrated by analysis of plasma after administration of a single 10 mg dose to 36 healthy subject. From the plasma rabeprazole concentration versus time curves, the mean $AUC_t$ (The area under the plasma concentration-time curve from time 0 to 12 hr ) was $691.36{\pm}321.88\;ng{\cdot}hr/mL$, $C_{max}$ (maximum plasma drug concentration) of $353.21{\pm}131.52\;ng/mL$ reached $3.4{\pm}1.1\;hr$ after adiministration. The mean biological half-life of rabeprazole was $1.37{\pm}0.75\;hr$. Based on the results, this simple method could readily be used in pharmacokinetics studies.

Study on Processing Methods to Remove Toxic Ptaquiloside from Bracken Fern (고사리의 독성물질 Ptaquiloside 제거방법 연구)

  • Lee, Hyang-Hee;Kim, Ae-Gyeong;Lee, Min-Gyou;Choi, Su-Yeon;Seo, Jin-Jong;Kim, Eun-Sun;Seo, Kye-Won;Cho, Bae-Sik
    • Journal of Food Hygiene and Safety
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    • v.32 no.3
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    • pp.217-221
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    • 2017
  • The ptaquiloside is a carcinogenic compound from bracken fern (Pteridium aquilinum L). This study was to evaluate the content of ptaquiloside in bracken fern by various processing methods. The processing methods were heated and immersed time, water exchange number, and so on. Akali hydrolysis and solvent fractionation of ptaquiloside in bracken fern leads to the non-toxic and chemically stable pterosin B. The contents of pterosin B was analyzed by UPLC-MS/MS on mobile phase 3 mM ammonium acetate and methanol. The contents of total pterosin B in non-processing bracken fern in water extraction was 81.0 mg/kg and toxic ptaquiloside of them was 46.4 mg/kg. The heating time of 5 minutes removed 60% about the contents of pterosin B in the bracken fern, and two-thirds of them were already non-toxic pterosin B, namely were not transfered from ptaquiloside. Additional immersed time (12h), the pterosin B in bracken fern was 10 mg/kg, it was removed 87.6% and once every hour, water exchange times were removed 99.5% in comparison with them of untreated bracken fern and two-thirds of them were non-toxic pterosin B. To remove of ptaquiloside in bracken fern, heat, immersion, and water exchange times shall be carried out simultaneously.

Production of Fungal Lipids (Part 2) Isolation of Starch Utilizing Mold and Its Optimum Compositions of Growth Media (곰팡이 유지 생산에 관한 연구 (제 2 보) 전분 이용성 곰팡이의 분리 및 배지조성에 관하여)

  • 신동화;김창식
    • Microbiology and Biotechnology Letters
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    • v.10 no.1
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    • pp.15-26
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    • 1982
  • A potential fungal lipid producer from starch, which was identified as Muror plumbeus, was isolated from natural sources and its optimum cultivation condition for lipid production was investigated. The Mucor plumbeus FRI 0007 showed the highest felt weight and lipid content which were 2.09 $\pm$ 0.24g per 50$m\ell$ of medium and 37.43% on dry weight basis respectively after 20 days incubation on the medium containing 21% of starch as a carbon source. The urea was the best nitrogen source as compared with sodium nitrate, potassium nitrate, magnesium nitrate, ammonium nitrate and ammonium acetate and its optimum concentration was 2.14g/$\ell$, showing 2.39 $\pm$ 0.07 g felt/50$m\ell$ of medium and 50.73% lipid content on dry weight basis after 25 days incubation. Besides the starch as a carbon source and urea as a nitrogen source, the Mucor plumbeus FRI 0007 utilized ZnSO$_4$, MgSO$_4$, NaH$_2$PO$_4$, $K_2$SO$_4$and FeCl$_3$as mineral sources. However, it did not require ail the above 5 minerals in group in-dispensably for its growth and lipid accumulation. The lipid and economic coefficient of Mucor plumbeus FRI 0007 grown on the medium containing 0.44g $K_2$SO$_4$or 5.00g MgSO$_4$/$\ell$solely were 14.96 and 15.37 and 31.12 and 26.10 which was higher than those on the medium containing the above 5 minerals.

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PHENOLOXIDASE AND ANTIOXIDANT IN KOREAN GINSENG (고려인삼에 있어서의 페놀 산화효소의 항산화물질)

  • Park E.Y.;Luh B.S.;Branen A.L.
    • Proceedings of the Ginseng society Conference
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    • 1984.09a
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    • pp.257-275
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    • 1984
  • Enzymatic browning is considered desirable in tea and tobacco processing but undesirable in many fruits processing at the present time. It is necessary to understand the nature of the enzyme, phenoloxidase, in order to control browning reactions, and extend its effects to formation of browning products as antioxidants in ginseng. Ginseng exhibits antioxidant activity when incorporated with turkey dark meat patties. The activity in red ginseng showed about two times stronger than white ginseng. One of the phenolic antioxidants from fresh, white and reprocessed white ginseng was identified as phenol 2.6 Bis(1.1 dimethyl ethyl) 4-methyl among several unknown compounds by GC/mass spectrometer. In red ginseng, no phenol 2.6 Bis (1.1 dimethyl ethyl) 4-methyl was detected, the compound may be polymerized by phenoloxidase and form some higher molecular compounds which may possess high antioxidant activity. Phenoloxidase isozymes in fresh Korean ginseng (panax ginseng C.A. Meyer) were extracted with phosphate buffer at pH 7.3. The isozymes were purified through ammonium sulfate fractionation, dialysis and chromatography on a DEAE-cellulose column. Two groups of phenoloxidase were shown to be present, one in the floating agglomerated group and the other in the precipitate. group from the 0.85 saturation ammonium sulfate. The DEAE-cellulose column chromatography, the phenoloxidase isozyme present in the precipitate appears as the first peak (I), and that in the agglomerate in the second peak (II). Isozyme I showed higher activity with catechin and catechal, and isozyme II showed higher activity with p-cresol. The isozyme showed two optimum pH activity one at pH 4.5 and the other at 8.5 with catechin as substrate. Korean ginseng phenoloxidase has high heat stability. When heated at $75^{\circ}C$ for 2 hours, its activity remained $90\%\;and\;80\%$ on phenoloxidase I and II respectively. Phenoloxidase I was most active on (+) catechin followed by p-cresal, catechol and epicatechin. Phenoloxidase II was most active on p-cresal followed by (+) catechin, catechol, p-coumanic acid and epicatechin. Sodium bisulfite, sodium cyanide, ascorbic acid glutachion in the oxidized form, sodium diethyl dithiocarbomate and ethylendiamine tetra acetate (EDTA) acted as inhibitors. Red ginseng color development was initiated by phenoloxidase and finished by a followed sun drying process. The antiaging activity of ginseng may be initiated by the antioxidant in the ginseng.

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Simultaneous Determination of Five Porphyrins in Human Urine and Plasma Using High Performance Liquid Chromatography-Tandem Mass Spectrometry

  • Hur, Yeoun;Tae, Sookil;Koh, Yun-Joo;Hong, Sung-Hyun;Yoon, Young Ho;Jang, Haejong;Kim, Sooji;Kim, Kyeong Ho;Kang, Seung Woo;Lee, Youngshin;Han, Sang Beom
    • Mass Spectrometry Letters
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    • v.5 no.2
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    • pp.42-48
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    • 2014
  • A specific and sensitive liquid chromatography-electrospray ionization tandem mass spectrometry method (LC-ESI-MS/MS) was developed and validated for the simultaneous quantification of porphyrins (coproporphyrin, pentacarboxylporphyrin, hexacarboxylporphyrin, heptacarboxylporphyrin, and uroporphyrin) in human plasma and urine. Acidified plasma samples and urine samples were prepared by using liquid-liquid extraction using ethyl acetate and protein precipitation with acetonitrile, respectively. The separation was achieved onto a Synergi Fusion RP column ($150mm{\times}2.0mm$, $4{\mu}m$) with a gradient elution of mobile phase A (0.1% formic acid in 2 mmol/L ammonium acetate, v/v) and mobile phase B (20% methanol in acetonitrile, v/v) at a flow rate of $450{\mu}L$/min. Porphyrins and the internal standard (IS), coproporphyrin I-$^{15}N_4$, were detected by a tandem mass spectrometer equipped with an electrospray ion source operating in positive ion mode. Multiple reaction monitoring (MRM) transitions of the protonated precursor ions and the related product ions were optimized to increase selectivity and sensitivity. The proposed method was validated by assessing selectivity, linearity, limit of quantification (LOQ), precision, accuracy, recovery, and stability. The calibration curves were obtained in the range of 0.1-100 nmol/L and the LOQs were estimated as 0.1 nmol/L for all porphyrins. Results obtained from the validation study of porphyrins showed good accuracy, precision, recovery, and stability. Finally, the proposed method was successfully applied to clinical studies on the autism spectrum disorder (ASD) diagnosis of 203 Korean children.

Studies on the cellulase properties of Aspergillus clavatus from the Cellulose-Cultural Properties (섬유질 문화재로부터 분리된 Aspergillus clavatus의 섬유소분해호소에 관한 연구)

  • Chung, Hee-Jin;Han, Sung-Hee;Ahn, Hee-Kyun;Min, Kyung-Hee
    • The Korean Journal of Mycology
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    • v.15 no.1
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    • pp.29-37
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    • 1987
  • Cellulolytic mocrooganisms were isolated from the cellulose-cultural properties. Among them, Aspergillus clavatus with the highest cellulase activity was identified by the morphological characteristics and it's enzyme activities were compared on the various cultural conditions. It was found that the induction of carboxymethylcellulase(CMCase), avicelase and salicinase in CMC liquid media showed the highest enzyme acitivity on five day's cultivation at $30^{\circ}C$ and thereafter their activities were gradually decreased with time. After crude extracellular enzymes precipitated with the 70% saturated ammonium sulfate solution were dialyzed with 20 mM acetate buffer pH 6.0, each crude enzyme was examined. The optimal activities of CMCase and avicelase were both found to be at $50^{\circ}C$ and pH 6.0. Their thermal stability was appeared at the $50^{\circ}C$. CMCase and avicelase had the maxima activities with 1.5% and 2.2% substrate concentration, respectively. The concentration of 5 mM $Mg^{++}$ or $Ca^{++}$ was found to have a maximum cellulase activity and its activity was inhibited with more than 5 mM $Cu^{++}$ and $Zn^{++}$ concentration. Cellulase activity was also inhibited sensitively by the inhibitors such as 2-mercaptoethanol, iodine and sodium azide.

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Optimization of solid phase extraction and simultaneous determination of trace anions in concentrated hydrofluoric acid by ion chromatography (불산 중 극미량 음이온 분석을 위한 고상 추출법 및 이온크로마토그래프를 이용한 동시분석법 확립)

  • Yoon, Suk-Hwan;Jo, Dong-ho;Kim, Hyun-Ji;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.29 no.5
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    • pp.219-224
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    • 2016
  • 불산 중 극미량 음이온의 고상추출과 이온크로마토그래프를 이용한 고감도 분석법이 개발되었다. 불산 중 불소이온이 고상에 의해 제거하였고 이어서 음이온 (F, CH3COO, Cl, Br, NO3, PO43−, SO42−)들이 이온크로마토그래프를 이용하여 연속적으로 분리하였다. 고상 추출법에 영향을 주는 각 인자들 (흡착제의 선택, 시료의 부피 및 pH, 용출 용액과 용출용액의 부피)을 결정하였으며 그 결과 흡착제로서 Oasis WAX 컬럼이 가장 우수하였고 1.0 mL의 시료부피, 용출용액으로 50 mM 초산암모늄염 5 mL가 분리능에서 가장 우수하였다. 개발한 방법에 의한 음이온 (Cl, Br, NO3, PO43−, SO42−)들의 방법검출한계는 25 % 불산용액 (w/w) 중에 0.04~0.30 µg/L의 범위를 보였고 정밀도는 20.0와 40.0 µg/L의 농도에서 5 % 이내를 보였다. 한 제조회사에 의한 25 % 불산 중 음이온의 4.2에서 47.5 µg/L의 범위로 모두 검출되었다. 이 방법은 시험절차가 간단하고, 재현성 및 감도가 좋아서 반도체회사에서 불산 중 음이온 불순물을 정도 관리하는데 매우 유용한 방법이 될 것으로 판단된다.