• Fisheries and Aquatic Sciences
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• v.25 no.2
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• pp.76-89
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• 2022

The Lophius litulon liver was used as raw material for the extraction of fish oil via various extraction methods. The extraction rate by water extraction, potassium hydroxide (KOH) hydrolysis and protease hydrolysis were compared and the results revealed the protease hydrolysis extraction had a higher extraction rate with good protein-lipid separation as observed by optical microscope. Furthermore, subsequent experiments determined neutrase to be the best hydrolytic enzyme in terms of extraction rate and cost. The extraction conditions of neutrase hydrolysis were optimized by single-factor experiment and response surface analysis, and the optimal extraction rate was 58.40 ± 0.25% with the following conditions: enzyme concentration 2,000 IU/g, extraction time 1.0 h, liquid-solid ratio 1.95:1, extraction temperature 40.5℃ and pH 6.5. The fatty acids composition in fish oil from optimized extraction condition was composed of 19.75% saturated fatty acids and 80.25% unsaturated fatty acids. The content of docosahexaenoic acid (DHA) and eicosapentaenoic acid (EPA) were 8.06% and 1.19%, respectively, with the ratio (6.77:1) surpassed to the recommendation in current researches (5:1). The results in this study suggest protease treatment is an efficient method for high-quality fish oil extraction from Lophius litulon liver with a satisfactory ratio of DHA and EPA.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.56 no.4
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• pp.428-437
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• 2023

A simultaneous analytical method was developed and validated for the analysis of prohibited fluoroquinolone (FQ) antibiotics including norfloxacin, ofloxacin, and pefloxacin, released by aquaculture in seawater and effluents. The samples were filtered, and extracts were obtained using a solid phase extraction cartridge with methanol (MeOH). The extracts were concentrated, and analyzed using ultra-performance liquid chromatography-tandem mass spectrometry. Two different columns and four different mobile phases were compared to achieve optimal separation and sensitivity for target compounds. Typical validation parameters including linearity, recovery of surrogate standard, instrument detection limit (IDL), limit of quantification (LOQ), and method detection limit (MDL) were evaluated. The linearity of calibration curves was over 0.999. Recoveries of surrogate ranged from 87.6% to 113%. The LOQ of target compounds was approximately 3-8 times lower than those reported in previous studies. The IDL and MDL were 0.06-0.57 and 0.06-0.37 ng/L, respectively. Seven effluent samples collected from an aquaculture located in Jeju were analyzed; however, not all target compounds were detected in the samples, suggesting that the banned antibiotics were not used. Overall, this established method was able to simultaneously analyze the three FQ antibiotics, and may be useful for monitoring prohibited antibiotics in the fishery industry.

• Journal of Animal Environmental Science
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• v.6 no.3
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• pp.175-184
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• 2000

A lab-scale MF membrane reactor was installed to investigate the membrane permeability, characteristics of membrane fouling at each conditions, and quality of permeate (liquid livestock manure) in the separation of solid-matters using membrane. Experiment was divided three filtration type such as follows; continuous filtration, gravity filtration, and intermittent filtration. As a result of experiment, flux 1 LMH was maintained for 7days, and trans-membrane pressure(TMP) was increased gradually under 10cmHg, but it was increased immediately after 10cmHg, respectively. However, the flux was increased, the Tmax was decreased exponential more and more. During the pure-flux test, most of the fouling of membrane was reversible. At the gravity filtration, permeate could be obtained as 1.75 LMH for 3.5days without any other electronic pressure. As an investigation of membrane surface, this study could be decided that the reason of fouling at the lower flux (Run 1 and 2) was attached matters in membrane surface, but at the higher flux (Run 4-6) was concentration polarization.

• Analytical Science and Technology
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• v.31 no.4
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• pp.171-178
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• 2018

Recently, for successful lactation, many breastfeeding mothers seek various products, including herbal medicine, dietary supplements, and prescribed medicines, to improve milk production. As demand for galactogogues grows, it is highly possible that pharmaceutical galactogogues may be adulterated with illegal products to maximize their efficacy. For continuous control and supervision of illegal products, we developed and validated a simple and sensitive LC-MS/MS method capable of simultaneously determining five galactogogues. Chromatographic separation was conducted using an Agilent Poroshell $120SB-C_{18}$ column with a mobile phase consisting of 20 mM ammonium formate (pH 5.4) and 100 % acetonitrile. The total run time was 13 min per analyte. The proposed method was performed according to the guidelines of the International Conference of Harmonization and it produced reliable results. This method showed high sensitivity and specificity, with a limit of detection (LOD) and limit of quantitation (LOQ) of 0.01-0.82 ng/mL and 0.02-2.45 ng/mL, respectively, for the solid- and liquid-type samples. Specificity was evaluated by analyzing matrix-blank samples spiked with the target compounds at LOQ levels, which provided a good separation of all peaks without interference. Additionally, the repeatability and intermediate precision were typically <15 %, whereas the recovery was 80-120 % of the values obtained using blank samples. Thus, we concluded that this method could be used for the identification and quantification of galactogogues in food or herbal products.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.13 no.10
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• pp.4927-4935
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• 2012

Turmeric is a medicinal herb with various pharmacological activities. Curcumin, demethoxycurcumin(DMC) and bisdemethoxycurcumin(BDMC) were extracted from turmeric by dipping and ultrasonic wave method. And extraction efficiency was identified using solid phase extraction(SPE). The extracted sample were simultaneously separated and analyzed from three kinds of commercial $C_{18}$ reversed-phase high performance liquid chromatography using water and acetonitrile as mobile phase with isocratic elution mode. Flow rate 1.0mL/min, injection volume $10{\mu}L$ and column oven temperature $40^{\circ}C$ at 425nm wavelength has been conducted. From the experimental results, the optimum mobile phase composition of water/acetonitrile 50/50vol% using RS tech column. It is evident that the amount of curcuminoids extracted(extraction time 4h) by 100% MeOH was higher than any aqueous MeOH composition. Finally, in 100% water extraction, the amount(mAU${\times}$mim) of curcuminoids extracted by SPE was 14.3 and 24.5 times respectively higher than ultrasonic wave and dipping method. The shown results can be applied as sources for pharmaceuticals and functional material.

• Analytical Science and Technology
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• v.14 no.3
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• pp.274-285
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• 2001

In this study, the thermal desorption-cryofocusing-gas chromatographic(TD-C-GC) method was developed for determination of volatile organic compounds(VOCs) in ambient air and was applied at the municipal solid waste landfill sites. On-column cryofocusing was possible only with a 100 ml dewars bottle in TD-C-GC method with a stainless steel column. However, high operating pressure was needed for purging VOCs from the absorbent trap, which was able to solve by pressure programming with a electric pressure controller. By using both pressure and temperature programming brought increasing of resolution power in on-column cryofocusing method, but the high pressure caused a leakage of sample tube with repeated use. A loop cryofocusing devise was also developed and compared with the direct on-column method. In loop cryofocusing method, VOCs were concentrated on a 0.8mm i.d. loop which is located between the injector and separation column by using liquid nitrogen. In order to purge VOCs from the absorbent trap, only 0.4 psi of pressure was need in the loop cryofocusing method. Dual detection system was applied for the analysis of VOCs; a FID was used for hydrocarbons and a FPD was used for sulfur-containing compounds. Qualitative analysis was done by on-column cryofocusing GC-MS system. Among the large number of VOCs, toluene was the most abundant. Hydrogen sulfide, dimethyl sulfide, carbon disulfide, dimethyl disulfide and methyl propyl disulfide were detected at landfill site by FPD.

• Korean Journal of Environmental Agriculture
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• v.35 no.3
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• pp.166-174
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• 2016

BACKGROUND: The current study developed a monitoring method of 6 veterinary antibiotics (amoxicillin, ampicillin, enrofloxacin, tetracycline, chlortetracycline, oxytetracycline) in agricultural soils using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive electrospray ionization mode.METHODS AND RESULTS: Sample preparation was carried out using acidic acetonitrile and citrate salts followed by purification with dispersive solid phase extraction (d-SPE). Separation on Eclipse Plus C₁₈ column was conducted in gradient of the mobile phase, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations expressed as the coefficient of determination was good with R²≥0.9900. The limit of quantifications (LOQs) ranged from 0.5 to 10 μg/kg for all analytes. Analysis of 51 agricultural soil samples taken in the Republic of Korea revealed concentrations less than 1.9 μg/kg for enrofloxacin, 75.5 μg/kg for chlortetracycline.CONCLUSION: The method was successfully applied to monitor 6 veterinary antibiotics from 51 field incurred agricultural soil samples in 17 provincial areas throughout the Republic of Korea. The developed method was simple, easy, and versatile and can be used for monitoring various veterinary antibiotics in soil.

• Journal of Korean Society of Environmental Engineers
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• v.30 no.9
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• pp.948-954
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• 2008

Membrane bioreactor(MBR) processes have been widely applied to wastewater treatment for last decades due to its excellent capability of solid-liquid separation. However, membrane fouling was considered as a limiting factor in wide application of the MBR process. Excess aeration into membrane surface is a common way to control membrane fouling in most MBR. However, the excessively supplied air is easily dissipated in the reactor, which results in consuming energy and thus, it should be modified for effective control of membrane fouling. In this study, cylindrical tube was introduced to MBR in order to use the supplied air effectively. Membrane fibers were immersed into the cylindrical tube. This makes the supplied air non-dissipated in the reactor so that membrane fouling could be controlled economically. Two different air supplying method was employed and compared each other; nozzle and porous diffuser which were located just beneath the membrane module. Transmembrane pressure(TMP) was monitored as a function of airflow rate, flux, and ratio of the tube area and cross-sectioned area of membrane fibers(A$_m$/A$_t$). Flow rate of air and liquid was regulated to obtain slug flow in the cylindrical tube. With the same flow of air supply, nozzle was more effective for controlling membrane fouling than porous diffuser. Accumulation of sludge was observed in the tube with the nozzle, if the air was not suppled sufficiently. Reduction of membrane fouling was dependent upon the ratio, A$_m$/A$_t$. For diffuser, membrane fouling was minimized when A$_m$/A$_t$ was 0.27, but 0.55 for nozzle.

• Resources Recycling
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• v.27 no.5
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• pp.61-68
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• 2018

The aluminum dross is oxide generated on the surface of the molten metal during the aluminum melting process and it is divided into white dross and black dross according to presence of the Salt flux. White dross has high metal content and is recycled via the melting process. Black dross is largely berried, because the it has a low metal content and difficulty in separating the components. Black dross contains a salt components such as NaCl and KCl, and inorganic materials such as $Al_2O_3$ and MgO, and it is necessary to study the technology to recover and recycle such valuable resources. In this study, a process for recycling aluminum black dross was proposed. The inorganic and soluble substances present in the black dross were separated through crushing-dissolution-solid/liquid separation-decompression evaporating. By controlling the ratio of water and black dross, the recovery condition of the separated product was optimized and we confirmed the highest Salt flux recovery efficiency 91 wt.% at black dross:water ratio 1:9. Finally, Through the synthesis of zeolite using recovered ceramic material, the materialization possibility of black dross was confirmed.

• Analytical Science and Technology
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• v.32 no.2
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• pp.35-47
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• 2019

In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak(R) C18 MG-II ($2.0mm{\times}100mm$, $3{\mu}m$), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with $R^2$ > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.