• Title/Summary/Keyword: liquid recovery

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Application of Three-phase Hollow Fiber LPME using an Ionic Liquid as Supported Phase for Preconcentration of Malachite Green from Water Samples with HPLC Detection

  • Zou, Yanmin;Zhang, Zhen;Shao, Xiaoling;Chen, Yao;Wu, Xiangyang;Yang, Liuqing;Zhu, Jingjing;Zhang, Dongmei
    • Bulletin of the Korean Chemical Society
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    • v.35 no.2
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    • pp.371-376
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    • 2014
  • A novel three-phase hollow fiber liquid phase microextraction was developed for the determination of malachite green (MG) in environmental waters, which selected [BMIM][$PF_6$] mixed with 1% trioctylphosphine oxide (TOPO) as supported phase. Several parameters (accepter phase pH, sample pH, supported phase membrane, volume of accepter phase, salinity, extraction time) that could affect extraction performance were investigated. Under the optimal extraction conditions, the established approach showed excellent characters as: high enrichment factor (212), wide linear range ($0.20-100{\mu}gL^{-1}$), low detection limit ($0.01{\mu}gL^{-1}$), good reproducibility (RSD, 8.9%, n=5) and satisfactory recovery (84.0-106.2%). The method was applied to detect MG at Yangtze River and pond waters in Zhenjiang, Jiangsu province, and 4 sites among 15 sampling sites were found MG with the concentration of $1.73-11.06{\mu}gL^{-1}$, which confirmed that the proposed environmentally friendly method was simple and effective for monitoring MG in aquatic system.

Determination of Patulin in Commercial Apple Juice in Korea by High Performance Liquid Chromatography (High Performance Liquid Chromatography를 이용한 국내 시판 사과 주스의 Patulin 분석)

  • Cho, Wan-Il;Choi, Young-Boong;Moon, Tae-Wha
    • Korean Journal of Food Science and Technology
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    • v.29 no.3
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    • pp.412-416
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    • 1997
  • Seven brands of commercial apple juice in Korea obtained from local stores were analyzed for patulin. Sep-Pak silica cartridge purification of the extract by ethyl acetate offered a good separation of patulin from other components. Patulin was determined by reverse phase liquid chromatography using a J'sphere $4\;{\mu}m$ ODS-H80 column with an ultraviolet detector set at 274 nm. Patulin concentrations in four samples ranged from 4 to $20\;{\mu}g/L$ and the other three samples from 30 to $45\;{\mu}g/L$. The limit of detection was $3\;{\mu}g/L$, and the recovery was $80{\sim}90%$ at the contamination level of $3.78{\sim}125.9\;{\mu}g/L$.

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Separation of Acetic Acid from Simulated Biomass Hydrolysates Containing Furans by Emulsion Liquid Membranes with an Organophosphorous Extractant (유기인산계 추출제를 이용한 에멀젼형 액막법에 의해 푸란유도체를 함유하는 모사 바이오매스 가수분해액으로부터 초산의 분리)

  • Lee, Sang Cheol
    • Korean Chemical Engineering Research
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    • v.56 no.5
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    • pp.687-693
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    • 2018
  • The selective removal and recovery of fermentation inhibitors during purification of sugars from biomass hydrolysates can increase the economic efficiency of the entire process to produce bioalcohol from lignocellulosic biomass. This study investigated the effect of furans in phenols-free biomass hydrolysate on acetic acid extraction in an emulsion liquid membrane system. Under specific operating conditions, more than 99% of acetic acid could be extracted within 5 minutes, and the degrees of extraction of furfural and 5-hydroxymethylfurfural were about 10% and 4%, respectively. The extraction rate of acetic acid was also lower at a higher initial concentration of furfural in the feed phase, which was greater for furfural than 5-hydroxymethylfurfural. Thus, if furfural is first removed from the hydrolysate prior to acetic acid extraction, emulsion liquid membrane would be a more economically efficient way of removing acetic acid.

Liquid chromatography-tandem mass spectrometric analysis of oleracone D and its application to pharmacokinetic study in mice

  • Lim, Dong Yu;Lee, Tae Yeon;Lee, Jaehyeok;Song, Im-Sook;Han, Young Taek;Choi, Min-Koo
    • Analytical Science and Technology
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    • v.34 no.5
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    • pp.193-201
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    • 2021
  • We have demonstrated a sensitive analytical method of measuring oleracone D in mouse plasma using a liquid chromatography-tandem mass spectrometry (LC-MS/MS). Oleracone D and oleracone F (internal standard) in mouse plasma samples were processed using a liquid-liquid extraction method with methyl tertbutyl ether, resulting in high and reproducible extraction recovery (80.19-82.49 %). No interfering peaks around the peak elution time of oleracone D and oleracone F were observed. The standard calibration curves for oleracone D ranged from 0.5 to 100 ng/mL and were linear with r2 of 0.992. The inter- and intra-day accuracy and precision and the stability fell within the acceptance criteria. The pharmacokinetics of oleracone D following intravenous and oral administration of oleracone D at doses of 5 mg/kg and 30 mg/kg, respectively, were investigated. When oleracone D was intravenously injected, it had first-order elimination kinetics with high clearance and volume of distribution values. The absolute oral bioavailability of this compound was calculated as 0.95 %, with multi-exponential kinetics. The low aqueous solubility and a high oral dose of oleracone D may explain the different elimination kinetics of oleracone D between intravenous and oral administration. Collectively, this newly developed sensitive LC-MS/MS method of oleracone D could be successfully utilized for investigating the pharmacokinetic properties of this compound and could be used in future studies for the lead optimization and biopharmaceutic investigation of oleracone D.

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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    • v.62 no.2
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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.

Liquid Chromatography-Tandem Mass Spectrometric Analysis of Nannozinone A and Its Application to Pharmacokinetic Study in Mice

  • Lee, Chul Haeng;Kim, Soobin;Lee, Jaehyeok;Jeon, Ji-Hyeon;Song, Im-Sook;Han, Young Taek;Choi, Min-Koo
    • Mass Spectrometry Letters
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    • v.12 no.1
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    • pp.21-25
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    • 2021
  • We aimed to develop and validate a sensitive analytical method of nannozinone A, active metabolite of Nannochelins A extracted from the Myxobacterium Nannocytis pusilla, in mouse plasma using a liquid chromatography-tandem mass spectrometry (LC-MS/MS). Mouse plasma samples containing nannozinone A and 13C-caffeine (internal standard) were extracted using a liquid-liquid extraction (LLE) method with methyl tert-butyl ether. Standard calibration curves were linear in the concentration range of 1 - 1000 ng/mL (r2 > 0.998) with the inter- and intra-day accuracy and precision results less than 15%. LLE method gave results in the high and reproducible extraction recovery in the range of 78.00-81.08% with limited matrix effect in the range of 70.56-96.49%. The pharmacokinetics of nannozinone A after intravenous injection (5 mg/kg) and oral administration (30 mg/kg) of nannozinone A were investigated using the validated LC-MS/MS analysis of nannozinone A. The absolute oral bioavailability of nannozinone A was 8.82%. Plasma concentration of nannozinone A after the intravenous injection sharply decreased for 4 h but plasma concentration of orally administered nannozinone A showed fast distribution and slow elimination for 24 h. In conclusion, we successfully applied this newly developed sensitive LC-MS/MS analytical method of nannozinone A to the pharmacokinetic evaluation of this compound. This method can be useful for further studies on the pharmacokinetic optimization and evaluating the druggability of nannozinone A including its efficacy and toxicity.

Control of Nano-Structure of Ceramic Membrane and Its Application (세라믹 멤브레인의 나노구조 제어 및 응용)

  • Lee, Hye-Ryeon;Seo, Bong-Kuk;Choi, Yong-Jin
    • Membrane Journal
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    • v.22 no.2
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    • pp.77-94
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    • 2012
  • Amorphous ceramic membranes have been developed for gas phase separation and liquid phase separation (water treatment, wastewater treatment and separation of organic solvent or compounds) because of their thermal stability and solvent resistance. In this paper, ceramic membranes were categorized by membrane pore size and materials, and summarized for hydrogen separation, carbon dioxide separation, membrane reactor, pervaporation and water treatment with membrane structure and properties.

Optimization of Extended UNIQUAC Parameter for Activity Coefficients of Ions of an Electrolyte System using Genetic Algorithms

  • Hashemi, Seyed Hossein;Dehghani, Seyed Ali Mousavi;Khodadadi, Abdolhamid;Dinmohammad, Mahmood;Hosseini, Seyed Mohsen;Hashemi, Seyed Abdolrasoul
    • Korean Chemical Engineering Research
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    • v.55 no.5
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    • pp.652-659
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    • 2017
  • In the present research, in order to predict activity coefficient of inorganic ions in electrolyte solution of a petroleum system, we studied 13 components in the electrolyte solution, including $H_2O$, $CO_2$ (aq), $H^+$, $Na^+$, $Ba^{2+}$, $Ca^{2+}$, $Sr^{2+}$, $Mg^{2+}$, $SO_4$, $CO_3$, $OH^-$, $Cl^-$, and $HCO_3$. To predict the activity coefficient of the components of the petroleum system (a solid/liquid equilibrium system), activity coefficient model of Extended UNIQUAC was studied, along with its adjustable parameters optimized based on a genetic algorithm. The total calculated error associated with optimizing the adjustable parameters of Extended UNIQUAC model considering the 13 components under study at three temperature levels (298.15, 323.15, and 373.15 K) using the genetic algorithm is found to be 0.07.

Determination of Ceftiofur in Bovine Serum by liquid Chromatography-Electrospray Mass Spectrometry (액체크로마토그래프/질량분석기를 이용한 소의 혈청 중 Ceftiofur의 분석)

  • Lim, Jong-hwan;Jang, Beon-su;Park, Byung-kwon;Yun, Hyo-in
    • Korean Journal of Veterinary Research
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    • v.43 no.3
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    • pp.429-433
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    • 2003
  • This study was aimed to develop a more rapid, simple and sensitive method to determine ceftiofur in bovine serum using LC/MS with electrospray interface. Separation was achieved on the Nova-Pak $C_{18}$ reverse phase column. The mobile phase consisted of 0.1% acetic add in water (A) and acetonitrile (B) and gradiently flowed at the rate of 0.4 mL/min. As a result of analysis of blank muscle samples, matrix interference was not shown. Limit of detection and limit of quantitaion was 5 ng/g and 20 ng/g, respectively. The values of precision and recovery satisfied the guideline of NVRQS. The precision and recovery developed in this method are suitable and sensitive to determine the concentration of ceftiofur in the bovine serum. These results could be applied for the confirmation and quantification in the biofluid.

Development of Analytical Method of Biotin in Complex Drugs and Dietary Supplements Using HPLC-UV

  • Huh, Yoon-Young;Kang, Yun-Pyo;Choi, Yong-Seok;Park, Jeong-Hill;Kwon, Sung-Won
    • Journal of Pharmaceutical Investigation
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    • v.41 no.1
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    • pp.25-30
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    • 2011
  • Recently, Korean Food and Drug Administration (KFDA) has focused on developing quality control guidelines for all commercial products in Korea to enforce regulations, improve the quality control, and protect consumers by developing prevalently used and efficient analytical tools to determine and quantify target compounds. Because the Korean Pharmacopeia (KP) presents microbiological assays for biotin, which is laborious and time-consuming, this study is focused on applying HPLC-UV to detect and quantify biotin in complex drugs and dietary supplements like multi-vitamin. Biotin in complex drugs was extracted from methanol and analyzed using mobile phase with 10 mM potassium phosphate (monobasic, pH=3.0) in distilled water and acetonitrile. Gradient condition was used to successfully detect and quantify biotin within 20 minutes. Validation result for linearity was significant that average $r^2$ was 0.999 (n=3) and its relative standard deviation (RSD) was 0.0578% which was less than 2%. Using this method, quantification of biotin in complex drugs was completed successfully and recovery tests were finished that recovery percentage greater than 95% with relative standard deviation less than 2%.