• Title/Summary/Keyword: liquid recovery

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Simultaneous analysis of sulfonamides in beef and pork by high performance liquid chromatography and electrospray ionization mass spectrometry (HPLC와 LC/MS에 의한 식육내 잔류 설파제의 동시 분석법)

  • 정봉수;박준조;금모래;김인경;박병옥;한정희
    • Korean Journal of Veterinary Service
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    • v.27 no.1
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    • pp.17-29
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    • 2004
  • A multiresidual analysis was performed to determine 12 sulfonamides(sulfacetamide, sulfadiazine, sulfisomidine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfisoxazole, sulfamethoxazole, sulfaquinoxaline, and sulfadimethoxine) in beef and pork simultaneously. The multiresidual analysis for the sulfonamides currently used was able to analyze 5 kinds of sulfonamides at the same time. The method of this 12 sulfonamides multiresidual analysis in this study was matrix solid-phase dispersion(MSPD) by high performance liquid chromatography (HPLC) and liquid chromatography mass spectrometry (LC/MS). The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM: Ethylacetate(3:1), DCM:EA(9:1). Also, samples (84 beef and 205 pork samples) which were positive by EEC-4 plate test from 2001 to 2003 were tested to investigate the kinds of sulfonamides using HPLC. The results from the study were as follows; 1. The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM:Ethylacetate(3:1), DCM:EA(9:1). The method of extraction solvent with DCM:ethyl acetate(9:1) was the most excellent(87.7∼99.3%) in separation and reappearance. 2. In the LC/MS analysis. of sulfonamides, signal to noise ratio was showed relatively high in the positive mode and special ion in the quality analysis was determined via [M+H]$\^$+/ and m/z 156. A spectrum of sulfonamides was showed from all 12 sulfonamides. 3. The samples positive by the EEC-4 plate, a screening test method, were categorized by sulfonamides through Charm II and confirmed the kinds of sulfonamides through HPLC. 1) Among 84 beef samples positive by EEC-4 plate, 20 samples were positive by Charm II and identified as 7 sulfamethazine, 9 sulfadimethoxine, 1 sulfamonomethoxine and 3 unknown status. 2) Among 205 pork samples positive by EEC-4 plate, 42 samples were positive by Charm II and identified as 19 sulfamethazine, 1 sulfadimethoxine, 4 sulfamonomethoxine and 5 unknown status.

Studies on the Elution Behavior and the Simultaneous Analysis of Some Metal-Dithiocarbamate Chelates by Reversed-Phase High Performance Liquid Chromatography (역상 액체 크로마토그래피에 의한 몇가지 금속-Dithiocarbamate 킬레이트의 용리거동 및 동시분석에 관한 연구)

  • Dai Woon Lee;Yun Je Kim;Hyun Chul Kim;Won Lee
    • Journal of the Korean Chemical Society
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    • v.32 no.3
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    • pp.211-226
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    • 1988
  • Liquid chromatographic behavior of several metal ions in dithiocarbamate(DTC) chelates were investigated by reversed phase high performance liquid chromatography on Novapak $C_{18}$ and ${\mu}$-Bondapak $C_{18}$ columns. The optimum conditions for the separation of DTC-metal chelate were examined with respect to the pH, shaking time, flow rate, extraction solvent, and mobile phase strength. The metal ions in mixtures at trace level, chelated with some dithiocarbamate derivatives were separated successfully on Novapak $C_{18}$ column using acetonitrile/methanol/water or acetonitril/water mixtures as mobile phases. It was found that all DTC metal chelates studied were eluted in an acceptable range of capacity factor values ($0{\leqq}log\;k'{\leqq}1$). Although several foreign metal ions were coexisted, high recovery and good precision were attained ; 97.0-106.7 % for the recovery and 0.98-3.41% for the coefficient of variation. Under the optimum analytical conditions, trace metal ions in the composite water samples were determined sucessfully with in relative error of about {\pm}$6.7 %.

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One-pot synthesis of silica-gel-based adsorbent with Schiff base group for the recovery of palladium ions from simulated high-level liquid waste

  • Wu, Hao;Kim, Seong-Yun;Ito, Tatsuya;Miwa, Misako;Matsuyama, Shigeo
    • Nuclear Engineering and Technology
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    • v.54 no.10
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    • pp.3641-3649
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    • 2022
  • A simple solvothermal reaction was used to prepare a 3-aminopropyl-functionalized silica-gel-based adsorbent for adsorbing Pd(II) from the nitric acid solution. Scanning electron microscopy, fourier transform infrared spectroscopy, and thermogravimetry analysis were performed on the as-synthesized adsorbent to demonstrate the successful introduction of Schiff base groups. Batch experiments were used to investigate the effects of contact time, nitric acid concentration, solution temperature, and adsorption capacity. It is worth noting that the prepared adsorbent exhibited a higher affinity toward Pd(II) with the uptake approximately 100% even in a 2 M HNO3 solution. At an equilibrium time of 5 h, the maximum adsorption capacity of Pd(II) was estimated to be 0.452 mmol/g. The adsorbed Pd(II) could be completely eluted by dissolving 0.2 M thiourea solution in 0.1 M HNO3. Using a combination of particle-induced X-ray emission analysis and an X-ray photoelectron spectrometer, the adsorbed Pd was found to be uniformly distributed on the surface of the prepared adsorbent and the existing species were Pd(II) and zero-valent Pd(0). Due to the desirable performances, facile preparation method, and abundant raw material source, the prepared adsorbent demonstrated a high application potential in the recovery of Pd(II) from simulated high-level liquid waste treatment.

Simultaneous detection for synthetic antimicrobials in muscle by high performance liquid chromatography-mass selective detector (HPLC-MSD) (HPLC-MSD 를 이용한 식육 중 합성항균제의 동시분석)

  • Hong In-Suk;Choi Yoon-Hwa;Kwon Taek-Boo;Lee Jung-Hark
    • Korean Journal of Veterinary Service
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    • v.29 no.3
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    • pp.317-330
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    • 2006
  • This study was conducted to develop the analytical method about simultaneous determination for synthetic antimicrobials in muscle by high performance liquid chromatography - mass selective detector (HPLC- MSD). Solid phase extraction (SPE), matrix solid phase dispersion (MSPD) and liquid-liquid extraction (LLE) have been adapted as pretreatment procedures for HPLC- MSD. Among various solvent tested, methanol was chosen for extraction of synthetic antimicrobials in muscles. For the optimized response, the values of various MS parameters including fragment voltage, drying gas flow, nebulizer pressure, drying gas temperature were verified. The average recovery rates using MSPD and SPE for muscles of bovine and pork were 78.9-127.1% and 78.3-121.7%, respectively. This method was verified the satisfactory performance for fourteen synthetic antimicrobials excepting carbadox in muscle of pork as detection limit of $0.05{\mu}g/g$ on API/ES SIM mode.

Determination of tylosin in edible meats by high-performance liquid chromatography (HPLC를 이용한 식육내 타이로신의 잔류분석법)

  • Kim, Gon-sup;Shin, Sun-hye;Kim, Jong-su;Ra, Do-kyung
    • Korean Journal of Veterinary Research
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    • v.41 no.1
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    • pp.13-19
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    • 2001
  • A simple and rapid analytical method for the determination of tylosin in chicken, pork and muscle was established by High-Performance Liquid Chromatography(HPLC). Chicken, pork and beef muscle(5 g) were fortified by adding the $0.2{\mu}g/ml$ of standard tylosin and the drug was extracted from meats with 70% acetonitrile(ACN) and followed by liquid-liquid partition for clean-up procedure. Then $20{\mu}l$ portion of ACN elution was directly analyzed by HPLC with spectra 100 variable wavelength detector, and unfortified blank control were treated similarly. The average recovery rate of tylosin added to chicken, pork and beef muscle were $83{\pm}2.3$, $96{\pm}3.3$ and $92{\pm}1.6$(%) at the level 0.2 ppm, respectively. No tylosin residues in marketing meats. These results suggested that HPLC methodology could be acceptable for the extraction, determination and screening of tylosin residues in edible meats.

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Rapid Quantification of Topotecan in Biological Samples by Liquid Chromatography/Tandem Mass Spectrometry

  • Shin, Beom-Soo;Lee, Mann-Hyung;Yoo, Sun-Dong
    • Journal of Pharmaceutical Investigation
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    • v.39 no.5
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    • pp.367-372
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    • 2009
  • A rapid liquid chromatography/tandem mass spectrometry (LC/MS/MS) assay method was developed for the determination of topotecan levels in rat serum. The assay utilized a single liquid-liquid extraction with a mixture of ethy l acetate and acetonitrile (6:1 v/v) and isocratic elution. The multiple reaction monitoring was based on the transition of m/z 422.0$\rightarrow$376.5 for topotecan and 315.1$\rightarrow$226.6 for clomipramine (internal standard). The developed assay was validated to demonstrate the specificity, recovery, lower limit of quantification (LLOQ), accuracy and precision. The assay was linear over a concentration range from 0.5-100 ng/mL, with LLOQ being 0.5 ng/mL using a small volume of rat serum (0.1 mL). The mean intra- and inter-day assay accuracy was 87.7-111.0% and 97.8-108.3, respectively, and the mean intra- and interday precision was between 1.6-4.3% and 3.8-10.3, respectively. The developed assay was applied to a pharmacokinetic study after a bolus i.v. injection of topotecan in rats.

Simultaneous Analysis of Pesticide Priority Pollutants in Water Samples (수질 시료 중의 Pesticide Priority Pollutants 동시분석에 관한 연구)

  • Kim Kye-Young;Kim Chong-Hyeak;Lee Sueg-Geun
    • Journal of the Korean Chemical Society
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    • v.37 no.6
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    • pp.590-598
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    • 1993
  • The simultaneous analysis of samples, 16 organic pesticides in water among 129 priority pollutants listed by EPA, was performed by GC-ECD (electron capture detector) and GC/MS-SIM (selected ion monitoring). Two extraction procedures, liquid-liquid extraction (LLE) and solid-phase extraction (SPE), were studied as an extraction and concentration method. Accuracy and precision of the methods were measured by the calculation of mean recovery and mean relative standard deviation. Finally, the detection limits, the experimental limitations, and prospects were discussed.

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Liquid Chromatographic Determination of Etofenprox Residues in Foods with Mass-Spectrometric Confirmation

  • Lee, Young-Deuk;Kwon, Chan-Hyeok;Kwon, Ki-Sung
    • Korean Journal of Environmental Agriculture
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    • v.30 no.4
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    • pp.432-439
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    • 2011
  • BACKGROUND: An official analytical method was developed to determine etofenprox residues in agricultural commodities using high-performance liquid chromatography (HPLC). METHODS AND RESULTS: The etofenprox residue was extracted with acetone from representative samples of five raw products which comprised rice grain, apple, mandarin, cabbage, and soybean. The extract was then serially purified by liquid-liquid partition and Florisil column chromatography. For rice and soybean samples, acetonitrile/n-hexane partition was additionally coupled to remove nonpolar lipids. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate etofenprox from co-extractives. Intact etofenprox was sensitively detected by ultraviolet absorption at 225 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine the etofenprox residue at 0.02 mg/kg. Mean recoveries from five crop samples fortified at three levels in triplicate were in the range of 93.6~106.4%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types. A selected-ion monitoring LC/mass spectrometry with positive atmospheric-pressure chemical ionization was also provided to confirm the suspected residue. CONCLUSION(s): The proposed method is simple, rapid and sensitive enough to be employed in routine inspection or monitoring of agricultural products for the etofenprox residue.

Performance Analysis of 1MW Organic Rankine Cycle with Liquid-Vapor Ejector using Effluent from Power Plant (화력발전소 폐열에 따른 작동유체별 액-증기 이젝터를 적용한 1MW급 ORC의 성능 분석)

  • Kim, Hyeon-Uk;Yoon, Jung-In;Son, Chang-Hyo
    • Journal of Power System Engineering
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    • v.18 no.6
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    • pp.120-125
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    • 2014
  • In this paper, suitable working fluid of 1MW Organic Rankine Cycle(ORC) with liquid-vapor ejector using effluent from power plant is selected. The results of comparison performance of 5 refrigerants are as follows; R600a, R134a, R1270, R236fa, R235fa. The operating parameters considered in this study include the condensation capacity evaporation capacity and efficiency. As a result of comparison of basic ORC system and with liquid-vapor ejector, with ORC system presents the higher system efficiency since the ejector makes the turbine outlet pressure lower than condensation pressure through its pressure recovery. Also, this ejector ORC system is advantageous in miniaturizing the size of components owing to decrease of evaporation capacity and condensation capacity.

Forage Yields of Corn-Oats Cropping System and Soil Properties as Affected by Liquid Cattle Manure (옥수수-연맥조합의 사초수량과 토양특성에 미치는 소 액상분뇨)

  • Shin, D.E.;Kim, D.A.;Park, G.J.;Kim, J.D.;Park, H.S.;Kim, S.G.
    • Journal of The Korean Society of Grassland and Forage Science
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    • v.19 no.4
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    • pp.325-332
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    • 1999
  • A manure management plan is important for all dairy operations. This experiment was conducted to determine the effect of different nitrogen(N) application rates of liquid cattle manure on the forage quality, N recovery, and total forage yields of corn-oats cropping system and soil properties at the National Livestock Research Institute, RDA, Suweon in 1997. Eight treatments consisting of no fertilizer, chemical fertilizer $320kg\;N\;ha^{-1}$ as urea, the continuous applications of 320, 640 and $960kg\;N\;ha^{-1}$ as liquid cattle manure(LCM), the residual effects of 200, 400 and $600kg\;N\;ha^{-1}$ as liquid cattle manure were arranged in a randomized complete block design with three replications. Mean plant height of fall sown oats was 70 and 61cm at the continuous application and the residual effect plots, respectively. Mean dry matter percent of fall sown oats at the residual effect plots was higher by 0.9% than that of oats at the continuous application plots, but there were no differences among all treatments. Mean crude protein(CP), acid detergent fiber(ADF), and neutral detergent fiber (NDF) contents of fall sown oats at the continuous application plots were higher by 1.0, 1.6, and 3.1%, respectively, than those of the residual effect plots. Also, there were significant differences among treatments (P<0.05). Total forage dry matter yields of corn and oats cropping system were ranged from 11,365 to $25,668kg\;ha^{-1}$ among the treatments. The yield was orderly ranked as LCM $960kg\;N\;ha^{-1}$ > LCM $600kg\;N\;ha^{-1}$ > LCM $640kg\;N\;ha^{-1}$ > LCM $400kg\;N\;ha^{-1}$ (P<0.05). Compared with the control, manurial value(MV) was 158 and 139% for the plot of the LCM $960kg\;N\;ha^{-1}$ and that of the LCM $600kg\;N\;ha^{-1}$, respectively. N recovery percent of fall sown oats was the highest at the plot of the LCM $200kg\;N\;ha^{-1}$ by 50%, and then was higher in order of the LCM $400kg\;N\;ha^{-1}$, LCM $600kg\;N\;ha^{-1}$, and LCM $320kg\;N\;ha^{-1}$. Contents of exchangeable cation in the soil of the residual effect plots was higher than that of the continuous application plots. These results suggest that the LCM $600kg\;N\;ha^{-1}$ may be the most effective in total forage dry matter yields, manurial value, N recovery, and utilizing liquid manure N under the corn and oats double cropping system.

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