• Title/Summary/Keyword: Selective recovery

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Development and validation of an LC-MS/MS method for determination of compound K in human plasma and clinical application

  • Kim, Jung Soo;Kim, Yunjeong;Han, Song-Hee;Jeon, Ji-Young;Hwang, Minho;Im, Yong-Jin;Kim, Jung Hyun;Lee, Sun Young;Chae, Soo-Wan;Kim, Min-Gul
    • Journal of Ginseng Research
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    • v.37 no.1
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    • pp.135-141
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    • 2013
  • A rapid, sensitive and selective analytical method was developed and validated for the determination of compound K, a major intestinal bacterial metabolite of ginsenosides in human plasma. Liquid-liquid extraction was used for sample preparation and analysis, followed by liquid chromatography tandem spectrometric analysis and an electrospray-ionization interface. Compound K was analyzed on a Phenomenex Luna C18 column ($100{\times}2.00$ mm, 3 ${\mu}m$) with the mobile phase run isocratically with 10 mM ammonium acetate-methanol-acetonitrile (5:47.5:47.5, v/v/v) at a flow rate of 0.5 mL/min. The method was validated for accuracy (relative error <12.63%), precision (coefficient of variation <9.14%), linearity, and recovery. The assay was linear over the entire range of calibration standards i.e., a concentration range of 1 ng/mL to 1,000 ng/mL ($r^2$ >0.9968). The recoveries of compound K after liquid-liquid extraction at 1, 2, 400, and 800 ng/mL were $106.00{\pm}0.08%$, $103.50{\pm}0.19%$, $111.45{\pm}5.21%$, and $89.62{\pm}34.46%$ for intra-day and $85.40{\pm}0.08%$, $94.50{\pm}0.09%$, $112.50{\pm}5.21%$, and $95.87{\pm}34.46%$ for inter-day, respectively. The lower limit of quantification of the analytical method of compound K was 1 ng/mL in human plasma. The developed method was successfully applied to a pharmacokinetic study of compound K after oral administration in ten of healthy human subjects.

Development and Validation of an HPLC Method for the Pharmacokinetic Study of Dipyridamole in Human (디피리다몰 체내동태 연구를 위한 혈청 중 디피리다몰의 HPLC 정량법 개발 및 검증)

  • Cho, Hea-Young;Kang, Hyun-Ah;Moon, Jae-Dong;Choi, Hoo-Kyun;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.36 no.1
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    • pp.45-51
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    • 2006
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of dipyridamole in human serum was developed, validated, and applied to the pharmacokinetic study of dipyridamole. Dipyridamole and internal standard, loxapine, were extracted from human serum by liquid-liquid extraction with diethyl ether and analyzed on a Nova Pak $C_{I8}$ column with the mobile phase of 40 mM ammonium acetate:methanol:acetonitrile (35:35:30)(v/v/v, pH 7.8). Detection wavelength of 280 nm and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed dipyridamole concentration (50 ng/mL) with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 2-2000 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 2 ng/mL, which was sensitive enough for pharmacokinetic studies of dipyridamole. The overall accuracy of the quality control samples ranged from 103.94 to 105.86% for dipyridamole with overall precision (% C.V.) being 4.60-11.49%. The relative mean recovery of dipyridamole for human serum was 97.64%. Stability studies showed that dipyridamole was stable during storage, or during the assay procedure in human serum. The peak area and retention time of dipyridamole were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of dipyridamole in human serum samples for the pharmacokinetic studies of orally administered Dimor tablet (75 mg as dipyridamole) at three different laboratories, demonstrating the suitability of the method.

Development and Validation of HPLC Method for Pharmacokinetic Study of Promethazine in Human (염산프로메타진 체내동태 연구를 위한 혈청 중 프로메타진의 HPLC 정량법 개발 및 검증)

  • Cho, Hae-Young;Kang, Hyun-Ah;Lee, Hwa-Jeong;Choi, Hoo-Kyun;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.36 no.1
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    • pp.23-29
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    • 2006
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of promethazine in human serum was developed, validated, and applied to the pharmacokinetic study of promethazine. Promethazine and internal standard, chlorpromazine, were extracted from human serum by liquid-liquid extraction with n-hexane containing 0.8% isopropanol and analyzed on a Capcell Pak CN column with the mobile phase of acetonitrile-0.2 M potassium dihydrogen phosphate (42:58, v/v, adjusted to pH 6.0 with 1 M NaOH). Detection wavelength of 251 nm and flow rate of 0.9 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed promethazine concentration (10 ng/mL) with respect to its peak area and retention time. In addition, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 1-40 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 1 mL of serum was 1 ng/mL, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 96.15 to 105.40% for promethazine with overall precision (% C.V.) being 6.70-11.22%. The relative mean recovery of promethazine for human serum was 63.54%. Stability (freeze-thaw and short-term) studies showed that promethazine was stable during storage, or during the assay procedure in human serum. However, the storage at $-80^{\circ}C$ for 4 weeks showed that promethazine was not stable. Extracted serum sample and stock solution were not allowed to stand at ambient temperature for 12 hr prior to injection. The peak area and retention time of promethazine were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of promethazine in human serum samples for the pharmacokinetic studies of orally administered Himazin tablet (25 mg as promethazine hydrochloride) at three different laboratories, demonstrating the suitability of the method.

cAMP induction by ouabain promotes endothelin-1 secretion via MAPK/ERK signaling in beating rabbit atria

  • Peng, Li-qun;Li, Ping;Zhang, Qiu-li;Hong, Lan;Liu, Li-ping;Cui, Xun;Cui, Bai-ri
    • The Korean Journal of Physiology and Pharmacology
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    • v.20 no.1
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    • pp.9-14
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    • 2016
  • Adenosine 3',5'-cyclic monophosphate (cAMP) participates in the regulation of numerous cellular functions, including the $Na^+-K^+$-ATPase (sodium pump). Ouabain, used in the treatment of several heart diseases, is known to increase cAMP levels but its effects on the atrium are not understood. The aim of the present study was to examine the effect of ouabain on the regulation of atrial cAMP production and its roles in atrial endothelin-1 (ET-1) secretion in isolated perfused beating rabbit atria. Our results showed that ouabain ($3.0{\mu}mol/L$) significantly increased atrial dynamics and cAMP levels during recovery period. The ouabain-increased atrial dynamics was blocked by KB-R7943 ($3.0{\mu}mol/L$), an inhibitor for reverse mode of $Na^+-Ca^{2+}$ exchangers (NCX), but did not by L-type $Ca^{2+}$ channel blocker nifedipine ($1.0{\mu}mol/L$) or protein kinase A (PKA) selective inhibitor H-89 ($3.0{\mu}mol/L$). Ouabain also enhanced atrial intracellular cAMP production in response to forskolin and theophyline ($100.0{\mu}mol/L$), an inhibitor of phosphodiesterase, potentiated the ouabain-induced increase in cAMP. Ouabain and 8-Bromo-cAMP ($0.5{\mu}mol/L$) markedly increased atrial ET-1 secretion, which was blocked by H-89 and by PD98059 ($30{\mu}mol/L$), an inhibitor of extracellular-signal-regulated kinase (ERK) without changing ouabain-induced atrial dynamics. Our results demonstrated that ouabain increases atrial cAMP levels and promotes atrial ET-1 secretion via the mitogen-activated protein kinase (MAPK)/ERK signaling pathway. These findings may explain the development of cardiac hypertrophy in response to digitalis-like compounds.

Monitoring of Butyltin Compounds in PVC Food Packaging - Determination of Butyltin Compounds in PVC Wrap and Gasket for Food Packaging by GC/MS (식품용 염화비닐수지제 기구 및 용기.포장 중 부틸주석화합물의 모니터링 - GC/MS를 이용한 염화비닐수지제 식품용 랩 및 가스킷 재질 중 부틸주석화합물 잔류량 분석)

  • Sung, Jun-Hyun;Yoon, Hae-Jung;Choi, Hyun-Cheol;Jeon, Dae-Hoon;Eom, Mi-Ok;Kim, Hyung-Il;Park, Na-Young;Lee, Eun-Joon;Lee, Young-Ja
    • Korean Journal of Food Science and Technology
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    • v.39 no.6
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    • pp.715-720
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    • 2007
  • The levels of butyltin compounds in poly(vinyl chloride) (PVC) food packaging using gas chromatography/mass spectrometry (GC/MS) were monitored. The analytical method, involving the ethylation with sodium tetraethylborate, was found to be selective and sensitive for mono-n-butyltin (MBT), di-n-butyltin (DBT), and tri-n-butyltin (TBT), validated by a $0.005\;{\mu}g/mL$ limit of detection (LOD), an $R^2>0.999$ for linearity, and >90% of recovery, respectively. Finally, none of the commercial food wraps and gaskets showed detectable levels of butyltin compounds.

Determination of Bisphenols Migrating from Epoxy Can Coatings to Aqueous Food Simulants (통조림관 코팅제에서 식품유사용매로 이행되는 비스페놀류의 분석)

  • Kang, Kyung-Mo;Shin, Hyo-Sun
    • Korean Journal of Food Science and Technology
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    • v.32 no.3
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    • pp.570-577
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    • 2000
  • A method was presented for determination of bisphenol F(BPF), bisphenol A(BPA), bisphenol F diglycidyl ether(BFDGE) and bisphenol A diglycidyl ether(BADGE) in 3 aqueous-based food simulants (water, 4% acetic acid, 20% ethanol) by reverse-phase high performance liquid chromatography(RP-HPLC)with fluorescence detection and gas chromatography with mass selective detection(GC/MSD). All the calibration lines in the range of $5{\sim}800\;{\mu}g/L$ had correlation coefficients greater than 0.9998 and detection limits of less than $1.2\;{\mu}g$ bisphenols/L. Precision at $200\;{\mu}g/L$ was under 3.1%. Recoveries of bisphenols simultaneously spiked to aqueous food simulants exceeded 95% for BPF and BPA but about 80% for BFDGE and BADGE. However, recoveris of BFDGE and BPADGE respectively spiked increased upto 95%. Detection limits in recovery test were less than $0.40\;{\mu}g$ bisphenols/L. In migration test bisphenols were determined by RP-HPLC coupled with confirmation by GC/MSD. Can coatings of epoxy phenol, modified epoxy, epoxy ester phenol and thermoset vinyl were exposed to the 3 aqueous food simulants. BPF, BFDGE and BADGE were not detected in all the can coatings but BPA was detected in 4% acetic acid and 20% ethanol in all the can coatings except modified epoxy.

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Removal/Recovery of VOCs Using a Rubbery Polymeric Membrane (Rubbery 고분가 막을 이용한 휘발성 유기화학물의 제거 및 회수)

  • Cha, Jun-Seok
    • Membrane Journal
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    • v.6 no.3
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    • pp.173-181
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    • 1996
  • Common volatile organic compounds(VOCs) such as toluene and methanol were removed successfully from N$_{2}$ using a novel silicone-coated hollow fiber membrane module. This novel membrane is a thin film composite(TFC) and was highly efficient in removing VOCs selectively from a N$_{2}$ stream. This membrane had some innate advantages over other silicone-based membrane in that the selective barrier was ultrathin(~1 $\mu$m) and the porosity of the polypropylene substrate was high which leads to a low permeation resistance. The substram was very strongly bonded to the coating layer by plasma polymerization and can withstand a very high pressure. A small hollow fiber module having a length of 25cm and 50 fibers could remove 96~99% of toluene as well as methanol vapors when the feed flow rate was up to 60cc/min. The percent removal of VOCs were even higher when the feed inlet concentration was higher. This process is especially suitable for treating streams having a low flow rate and high VOCs concentration. The permeances of VOCs through this membrane was in the range of $4~30 \times 10^{-9}gmol/sec \cdot cm^{2}\cdot cmHg$ for both toluene and methanol, and nitrogen permeance was between $3~9 \times 10^{-10}gmol/sec \cdot cm^{2} \cdot cmHg$. High separation factor between 10~55 for toluene/N$_{2}$ and 15~125 for methanol/N$_{2}$ were obtained depending on the feed flow rate ranges and feed VOCs concentration levels.

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Studies on the New Analytical Methods for Separation and Recovery of Rare Earth Metals (I) : Adsorption Characteristics of U(VI) Ion by New Synthetic Resins with Macrocyclic Compounds (희토류금속 분리 및 회수를 위한 분석화학적 연구 (제1보) : 우라늄(VI)의 분리회수를 위한 선택이온교환수지 합성과 우라늄(VI) 금속이온의 흡착특성)

  • Jung Oh Jin;Hak Jin Jung;Joon Tea Kim
    • Journal of the Korean Chemical Society
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    • v.32 no.4
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    • pp.358-370
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    • 1988
  • Several new ion exchange resins have been synthesized from chloromethyl styrene-1,4-divinylbenzene(DVB) with 1%, 2%, 4%, and 10%-crosslinking and macrocyclic ligands of cryptand type by interpolymerization method. The adsorption characteristics and the pH, time, solvents and concentration dependence of the adsorption of metal ions by this resin were studied. The correlation between the separation characteristics of uranium, rare earths and transition metal on the resins and the stability constants of complexes with macrocyclic ligands have been examined. The resins were very stable in both acidic and basic media and have good resistance to heat at $280^{\circ}C$. The $UO_2^{+2}$ aqueous solution are not adsorbed on the resins below pH 3.0, but the power of adsorption of $UO_2^{2+}$ increased rapidly above pH 4.0. The optimum equilibrium time for adsorption of metallic ions was twenty minutes and adsorptive power decreased in proportion to crosslinking size of the resins and order of dielectric constants of solvents used and the selective sequence for metal cations is in the order of $UO_2^{2+},\;Cu^{2+}\;and\;Nd^{3+}$.

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A Development of Active Monitoring and Approach Alarm System for Marine Buoy Protection and Ship Accident Prevention based on Trail Cameras and AIS (해상 부이 보호 및 선박 사고 예방을 위한 트레일 카메라-AIS 연계형 능동감시 및 접근경보 시스템 개발)

  • Hwang, Hun-Gyu;Kim, Bae-Sung;Kim, Hyen-Woo;Gang, Yong-Soo;Kim, Dae-Han
    • Journal of the Korea Institute of Information and Communication Engineering
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    • v.22 no.7
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    • pp.1021-1029
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    • 2018
  • The marine buoys are operated in various domains, which are navigation route and danger maker, weather and environment monitoring, military strategical element, etc. If the marine buoy is damaged, there consumes many cost and time for recovery or replacement, because of severe environmental condition, and causes a risk possibility of secondary accident. In this paper, we developed an active monitoring and approach alarm providing system using trail cameras and AIS for protection for the marine buoys. To do this, we analyzed existing researches and similar systems, extracted requirements for enhancement, and designed the system architecture that applied the enhanced elements. The main considerations of system enhancement are: integration of AIS and trail cameras, adopting of phased alarm technique by approaching ships, applying of selective communication module, conducting the image processing of ships for providing alarm, and applying thermal cameras. After that, we developed the system using designed architecture and verified effectiveness of the system based on laboratory or field-level tests.

Leaching of Vanadium and Tungsten from Spent SCR Catalysts for De-NOx by Soda Roasting and Water Leaching Method (소다배소(焙燒) 및 수침출법(水浸出法)에 의한 탈질용(脫窒用) 폐(廢) SCR 촉매(觸媒)로부터 바나듐과 텅스텐 침출(浸出))

  • Kim, Hye-Rim;Lee, Jin-Young;Kim, Joon-Soo
    • Resources Recycling
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    • v.21 no.6
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    • pp.65-73
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    • 2012
  • Selective catalytic reduction(SCR) catalysts are obtained from de-NOx system of thermoelectric power plant. A process was developed for valuable metals such as vanadium and tungsten recovery from spent SCR catalyst by using soda roasting followed by water leaching. Spent SCR catalyst having $V_2O_5$(1.23 mass %) and $WO_3$(7.73 mass %). For getting soluble metal forms of the targeted metals like vanadium and tungsten soda roasting process was implemented. In soda roasting process, sodium carbonate added 5 equivalent ratio at roasted temperature $850^{\circ}C$ with 120 min roasted time for $544{\mu}m$ particle size of spent SCR catalyst. After soda roasting process moved to water leaching for roasted spent catalyst. Before leaching process the roasted spent catalyst was grinded up to $-45{\mu}m$ size. The leaching time is 30 min at $40^{\circ}C$ temperature, 10 % pulp density. The final leaching efficiency obtained 46 % of vanadium and 92 % of tungsten from present process.