• Title/Summary/Keyword: 암모늄아세테이트법

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Applied-Mineralogical Characterization and Assessment of Some Domestic Bentonites (I): Mineral Composition and Characteristics, Cation Exchange Properties, and Their Relationships (국내산 벤토나이트에 대한 응용광물학적 특성 평가 (I): 광물 조성 및 특징과 양이온 교환특성과의 연계성)

  • 노진환
    • Journal of the Mineralogical Society of Korea
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    • v.15 no.4
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    • pp.329-344
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    • 2002
  • Mineralogical and chemical characterization of some domestic bentonites, such as quantitative XRD analysis, chemical leaching experiments, pH and CEC determinations, were done without any separation procedures to understand their relationships among mineral composition, characteristics, and cation exchange properties. XRD quantification results based on Rietveld method reveal that the bentonites contain totally more than 25 wt% of impurities, such as zeolites, opal-CT, and feldspars, in addition to montmorillonite ranging 30~75 wt%. Cation exchange properties of the zeolitic bentonites are deeply affected by the content of zeolites identified as clinoptilolite-heulandite series. Clinoptilolite is common in the silicic bentonites with lighter color. and occurs closely in association with opal-CT. Ca is mostly the dominant exchangeable cation, but some zeolitic bentonites have K as a major exchangeable cation, The values of cation exchange capacity (CEC) determined by Methylene Blue method are comparatively low and have roughly a linear relationship with the montmorillonite content of the bentonite, though the correlated data tend to be rather dispersed. Compared to this, the CEC determined by Ammonium Acetate method, i.e.‘Total CEC’, has much higher values (50~115 meq/100 g). The differences between those CEC values are much greater in zeolitic bentonites, which obviously indicates the CEC increase affected by zeolite. Other impurities such as opal-CT and feldspars seem to affect insignificantly on the CEC of bentonites. When dispersed in distilled water, the pH of bentonites roughly tends to increase up to 9.3 with increasing the alkali abundance, especially Na, in exchangeable cation composition. However, some bentonites exhibit lower pH (5~6) so as to regard as ‘acid clay’. This may be due to the presence of $H^{+}$ in part as an exchangeable cation in the layer site of montmorillonite. All the works of this study ultimately suggest that an assesment of domestic bentonites in grade and quality should be accomplished through the quantitative XRD analysis and the ‘Total CEC’measurement.

Preparation of Protein Adsorptive Anion Exchange Membrane Based on Porous Regenerated Cellulose Support for Membrane Chromatography Application (단백질 흡착성을 갖는 막 크로마토그래피용 재생 셀룰로오스 기반 음이온 교환 다공성 분리막의 제조)

  • Seo, Jeong-Hyeon;Lee, Hong-Tae;Kim, Tae-Kyung;Cho, Young-Hoon;Oh, Taek-Keun;Park, HoSik
    • Membrane Journal
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    • v.32 no.5
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    • pp.348-356
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    • 2022
  • With the development of the bio industry, membrane chromatography with a high adsorption efficiency is emerging to replace the existing column chromatography used in the downstream processes of pharmaceuticals, food, etc. In this study, through the deacetylation reaction of two commercial cellulose acetate (CA) membranes with different pore sizes, the porous regenerated cellulose (RC) supports for membrane chromatography were obtained to attach the anion exchange ligands. The adsorptive membranes for anion exchange were prepared by attaching an anion exchange ligand ([3-(methacryloylamino) propyl] trimethylammonium chloride) containing quaternary ammonium groups on the RC supports by grafting and UV polymerization. The protein adsorption capacities of the prepared membranes were obtained through both the static binding capacity (SBC) and the dynamic adsorption capacity (DBC) measurement. As a result, the membrane chromatography with the smaller the pore size, the larger the surface area showed the highest protein adsorption capacity. Membrane chromatography which was prepared by using deacetylated commercial CA support with MAPTAC ligand (i.e., RC 0.8 + MAPTAC: 43.69 mg/ml, RC 3.0 + MAPTAC: 36.33 mg/ml) showed a higher adsorption capacity compared to commercial membrane chromatography (28.38 mg/ml).

Study of Utilization of Natural Zeolites as Functional Materials for Water Purification (I): Cation Exchange Property of Domestic Zeolites (천연 제올라이트의 수환경 개선용 기능성 소재로의 활용에 관한 연구 (I): 국내산 제올라이트의 양이온 교환 특성)

    • Journal of the Mineralogical Society of Korea
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    • v.16 no.2
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    • pp.135-149
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    • 2003
  • Domestic zeolite ores are mostly composed of Ca-type clinoptilolite, accompanying a little amounts of mordenite. However, other types of zeolite ores rich in ferrierite, heulandite, or mordenite are less commonly found. Based on the quantitative XRD analysis, zeolite contents are determined to be nearly 50∼90 wt%. Impurities (mostly > 10 wt%) in the zeolite ores chiefly consist of quartz, feldspar, smectite, and opal-CT. The determined CEC values ($CEC_{AA}$ ) of powdery samples (grain size: < 125 $\mu\textrm{m}$) of zeolite ores by the Ammonium Acetate method are mostly higher than 100 meq/100 g. Some zeolites from the Guryongpo area, corresponding to the clinoptilolite ore, are measured to be dominantly high in CEC values ranging 170∼190 meq/100 g. Cation exchange property of the zeolite ores varies greatly depending on the types or zeolite species present in the ores. Despite of the lower grade in zeolite content, the $CEC_{AA}$ of ferrierite ore is comparatively high. Compared to this, the $CEC_{AA }$ of heulandite ore is very low, though the zeolite ore exhibits the highest grade ranging up to about 90 wt%. In addition, the CEC values calculated theoretically from the framework composition of clinoptilolite-heulandite series are not consistent with those determined by the cation exchage experiment. The measured $CEC_{AA}$ of clinoptilolite ores are generally higher than those of heulandite ores. This may be due to the higher Ca abundance in exchangeable cation composition and the presence of probable stacking faults in heulandite. The variation of $CEC_{CEC}$ is roughly proportional, though not strictly compatible, to the zeolite contents in clinoptilolite ores. It seems to be caused by the fact that the $CEC_{AA}$ of clinoptilolite locally varies depending on crystal-chemical diversity, i. e., the variation in framework composition (Si/Al) and exchangeable cation composition (especially, the contents of Ca and K). In addition, the determined CEC values ($CEC_{MB}$ ) of zeolite ores by the Methylene Blue method are much higher than those calculated from smectite contents. It suggests a probable reaction of Methylene Blue ion ($C_{16}$ $H_{18}$ $N_3$S+) with larger-pore zeolites than clinoptlolite-heulandite series, i.e., ferrierite and mordenite as well as with smectite. This can be supported by the fact that the ferrierite ore accompanying little amount of smectite has the highest value in CE $C_{MB}$ .

Development and Validation of the Determination of Sorafenib in Human Plasma using Tandem Mass Spectrometry Coupled with Liquid Chromatography (고속액체크로마토그래피 텐덤질량분석기법을 이용한 사람 혈장 내 소라페닙 농도분석법의 개발 및 검정)

  • Park, Daejin;Lee, Sunggon;Kim, Woomi
    • Journal of Life Science
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    • v.22 no.11
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    • pp.1456-1462
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    • 2012
  • Sorafenib is a multikinase inhibitor and an oral anticancer drug approved for the treatment of patients with advanced renal cell carcinoma and those with unresectable hepatocellular carcinoma. The purpose of this study was to develop an efficient method of the determination of sorafenib in human plasma using tandem mass spectrometry coupled with liquid chromatography (LC/MS/MS) and validate the method by the guidelines of the Korean Food and Drug Administration (KFDA). Plasma samples ($100{\mu}l$) were added with chlorantraniliprole as an internal standard and then mixed with the 0.1% formic acid-containing extraction solution composed of isopropyl alcohol and ethyl acetate (1:4, v/v). After centrifugation, the supernatant was concentrated at $45^{\circ}C$ under negative pressure and centrifugal force. The residue was reconstituted with a mobile phase and injected into the HPLC instrument using a reverse phase Waters XTerra$^{TM}$ C18 column (particle size $3.5{\mu}m$). Liquid chromatography was carried out within the run time of 5 min using a mobile phase composed of buffer (0.1% formic acid and 10 mM ammonium formate), methanol, and acetonitrile (1:6:3, v/v/v). The analytes were monitored by tandem mass spectrometry in the multiple reaction monitoring method programmed to detect sorafenib at 'm/z 465.2 ${\rightarrow}$ 252.5' and chlorantraniliprole at 'm/z 484.4 ${\rightarrow}$ 286.2' with positive electrospray ionization mode ($ES^+$). The result showed the proper linearity ($r^2$ > 0.99) over the range of 2,000-5,000 ng/ml with good accuracy (90.7-103.9%) and precision (less than 10%). The newly developed method using LC/MS/MS was validated by the guideline of KFDA and identified as more sensitive compared to the previous methods.

Studies on the Separation and Discrimination of the Natural Yellow Pigment on Croaker (참조기 천연색소의 분리 및 판별법에 관한 연구)

  • Kim, Hee-Yun;Hong, Ki-Hyung;Hong, Jin-Hwan;Kim, Dong-Sul;Han, Sang-Bae;Lee, Eun-Ju;Lee, Jeung-Seung;Kang, Kil-Jin;Chung, Hyung-Wook;Song, Kyung-Hee;Park, Jong-Seok;Kwon, Yong-Kwan;Jang, Young-Mi;Shin, Il-Shik;Lee, Chang-Kook;Park, Hee-Yul;Ha, Sang-Chul;Jo, Jae-Sun;Park, Hye-Kyung
    • Korean Journal of Food Science and Technology
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    • v.34 no.5
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    • pp.762-769
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    • 2002
  • As a preliminary test for defining intact yellow croaker pigment, the pigment was analyzed by column chromatography and UV-vis spectrophotometry. All maximum absorbance wavelengths commonly showed three maximum absorbance ranges, similar to those of carotenoid, suggesting that the tested pigment may be carotenoid. We detected total six peak RT values in the chromatogram through PDA-HPLC under gradient mode (behavior A at 10% for initial 2 min and changed to behavior B for 60 min). Most pigments were detected at the peak with 3.27 RT value. Because seven peaks were detected under gradient mode and three under isocratic mode [methanol : methylene chloride (90 : 10, v/v)], gradient mode was determined to be more appropriate for quantitative analysis. By the comparison test of RT values among yellow pigment in croakers and reference pigments, such as zeaxanthine, ${\beta}-cryptoxanthine$, ${\beta}-carotene$, and astaxanthin, only ${\beta}-cryptoxanthine$ was detected in the white croaker, whereas such pigment of yellow croaker having RT value of 31.02 was not detected. Therefore, RT value was found to be applicable for detecting adulterated croaker.