• Analytical Science and Technology
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• v.37 no.4
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• pp.211-219
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• 2024

This study presents a sensitive and reliable method for determining tetracycline (TC), oxytetracycline (OTC), and chlortetracycline (CTC) residues in shrimp samples. A two-step process involving liquid-liquid extraction (LLE) followed by solid-phase extraction (SPE) was developed prior to HPLC analysis. The target analytes were effectively extracted using EDTA/McIlvaine buffer (pH 4.0): methanol (80:20, %v/v), with subsequent clean-up using a C18 SPE cartridge. HPLC separation was conducted on a C18 column (250 mm × 4.6 mm i.d., 5 ㎛) at 30 ℃, using 0.01 % trifluoroacetic acid (A) and acetonitrile (B) as the mobile phase. A gradient elution protocol was applied, transitioning from 85(A):15(B) %v/v to 70(A):30(B) %v/v at 7 min, with a 5 min hold, followed by adjustment to 85(A):15(B) %v/v for 13-14 min. The detection was performed using photodiode array (PDA) at 365 nm with a flow rate of 1.0 mL/min. The calibration curves exhibited good linearity within a concentration range of 0.4-6.0 ㎍/mL (R² > 0.995). The limits of detection (LOD) for TC, OTC, and CTC in shrimp were 0.034, 0.029, and 0.021 ㎍/mL, respectively. The limits of quantitation (LOQ) for TC, OTC, and CTC were found to be 0.114, 0.097, and 0.071 ㎍/mL, respectively. Recoveries of TC, OTC, and CTC from spiked shrimp samples ranged from 91.0 % to 95.5 %, 92.4 % to 97.2 %, and 93.3 % to 96.6 %, respectively. This method was successfully applied to the determination of TC, OTC, and CTC residues in shrimp samples sourced from various local markets.

• Clean Technology
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• v.20 no.4
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• pp.349-353
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• 2014

Succinic acid is an important precursor in industries producing biopolymers, pharmaceutical and food additives and green solvents. However, due to the high price of petroleum and the global $CO_2$ emission, the biological production of succinic acid from renewable biomass is a novel process due to the fixation of $CO_2$ into succinate during fermentation. In this study, aqueous two phase systems based on imidazolium ionic liquids/$K_2HPO_4$ were used as an effective separation and concentration process for succinic acid. Experimental results show that aqueous two phase systems can be formed by adding appropriate amount of imidazolium ionic liquids to aqueous $K_2HPO_4$ solutions in the presence of succinic acid. It can be found that the ability of imidazolium ionic liquids for phase separation followed the order [HMIm][Br]${\fallingdotseq}$[OMIm][Br]>[BMIm][Br]>[EMIm][Br]. The maximum value of extraction efficiency for succinic acid was about 90% and the amount of coextracted water into top phase is proportional to the chain length of cation in imidazolium ionic liquids. It was concluded that the aqueous two phase systems composed of imidazolium ionic liquids/$K_2HPO_4$ was effective for the selective extraction and concentration of succinic acid.

• Korean Chemical Engineering Research
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• v.51 no.5
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• pp.575-579
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• 2013

1,3-Propandiol is a promising chemical which can be produced from fermentation of glycerol because the application of 1,3-propanediol is mainly in the production of bio-polytrimethylene terephthalate (bio-PTT). However, the cost of downstream processes in the biological production of 1,3-propanediol can make a high portion in the total production cost due to the large amount of water and the by-produced carboxylic acids such as succinic, lactic and acetic acids in 1,3-propanediol fermentation broth. In this study, aqueous two-phases systems composed of hydrophilic alcohols and phosphate salts were applied to the recovery of 1,3-propanediol from its artificial aqueous solution. Formation of aqueous biphases in hydrophilic alcohols and phosphate salts was due to the salting-out effect of salts in bottom phase, thereby 1,3-propanediol in bottom phase was moved into top phase. Extraction efficiency for 1,3-propanediol was proportional to the polarity of hydrophilic alcohols and the basicity of salts and the maximum value of extraction efficiency was more than 98%. In the aqueous two-phases systems after extraction, there was no carboxylic acid in top phase. Therefore, it was concluded that the aqueous two-phases systems composed of hydrophilic alcohols and phosphate salts were effective for the selective recovery of 1,3-propanediol without any coextraction of carboxylic acids.

• Journal of Korean Society on Water Environment
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• v.24 no.6
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• pp.801-805
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• 2008

A fibrous material (p-phenylene-2,5-benzobisoxazole, PBO) was used as an adsorbent for solid phase extraction in order to simplify the extraction procedure. The extraction performance for di-(2-ethylhexyl) phthalate (DEHP) was examined with two types of PBO fibers (HM (High modulus) and AS (Regular type) types) by batch type sorption/desorption experiments. When 100 mg of the HM fibers were applied to 20 mL of the aqueous DEHP solution (less than $50{\mu}g/L$), more than 95% of DEHP was adsorbed on the fibers, however, the AS type fibers adsorbed alkyl phthalate up to 80%. In the case of $50{\mu}g/L$ of the initial concentration of DEHP, the adsorbed DEHP was extracted effectively with methanol and the maximum overall recovery ratio was 92.3%. The results indicated that the PBO fibers could be used as an adsorbent for alkyl phthalate analysis, and that the extraction procedure was not affected by suspended solids in a water sample.

• Journal of the Korean Ceramic Society
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• v.18 no.4
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• pp.257-261
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• 1981

The tendency of glass containing titanium-dioxide to separate into two phases can be attributed to a change of the coordination number of titanium from six to four on increase of temperature and to "freezing" of the high temperature four fold coordination on cooling of the melt. Addition of TiO2 to the basic glass 8.7 $Na_2O$ 22.4B2O3 68.9 $SiO_2$ was varied 5 to 25 parts. The phase separation in the temperature range of transformation was examined with each heating temperature and soaking time. As the experimental results, the most distinct phase separation were obtained from alkali extraction method when $TiO_2$ was added 15 parts. The apparant activation energy was 30.5 Kcal/mole by alkali extraction method derived from Arrhenius plots.ius plots.

• Journal of the Korean Society of Tobacco Science
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• v.28 no.2
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• pp.152-157
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• 2006

A new procedure has been developed for the quantitation of aromatic amines in mainstream cigarette smoke. Two solid-phase extraction (SPE) clean up steps, using a different retention mechanisms, are required to process the samples. The first step used a cation-exchange cartridge, followed by a second step that used a cartridge with a hydrophobic retention character. The aromatic amines eluted from the second SPE cartridge are derivatized with pentafluoropropionic anhydride. This new method have advantages over other reported techniques, being sensitive, robust, and easily automated. The detection limits were ranged from 0.12 ng/mL for 1-aminonaphthalene to 0.16 ng/mL for 3-aminobiphenyl and the recoveries were from 97 to 106%. Compared with other reports for analysis of 2R4F reference cigarette, this method shows a close analytical data and good repeatability.

• Resources Recycling
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• v.17 no.3
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• pp.29-34
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• 2008

Solvent extraction behaviors of iron(III) from chloride solution at high ionic strength condition between Alamine336 and TBP were compared by using MaCabe-Thiele diagram. Extraction isotherms of iron by the two extractants were obtained by calculating the equilibrium concentrations of iron in both phases from the initial extraction conditions. In calculating the equilibrium concentration of iron, chemical equilibria in the aqueous phase and mass balance together with the solvent extraction reaction were considered. MaCabe-Thiele diagram of iron by 1M Alamine336 indicated that two extraction stages could lead to complete extraction of 0.5M iron from 3M HCl solution at an A/O ratio of 6/5. The extraction power of 1M Alamine336 was found to be the same as 2-3M TBP. MaCabe-Thiele diagram together with the physical properties of the two extractants indicated that Alamine336 is superior to TBP in extracting ferric iron from chloride solution.

• Proceedings of the Korean Institute of IIIuminating and Electrical Installation Engineers Conference
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• 2007.05a
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• pp.117-119
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• 2007

We need two operation modes to obtain the complex hologram without bias and the conjugate image in the modified triangular interferometer(MTI). To solve the problem, we proposed the optimized MTI with one wave plate, which can obtain cosine and sine functions by the combination of one wave plate and one linear polarizer. In the extraction of phase term using the combination of polarization components, the phase error occurs, and we analyzed such potential phase errors in the optimized MTI.

• Journal of the Korean Applied Science and Technology
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• v.34 no.4
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• pp.954-961
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• 2017

We investigated the purifications of PE-gal and CPN-gal, synthesized by transgalactosylation reaction using recombinant ${\beta}$-gal. The reaction mixture containing PE and PE-gal was first mixed with EA, and thereafter PE and PE-gal were distributed in two-phase (EA/water) system. In this system, PE and PE-gal was selectively moved into EA and water phase, respectively. Then, the water phase was collected, and silica gel chromatography was carried out using the collected water phase. Finally, we compared two purified PE-gal samples using HPLC and TLC analysis, in which the one was purified only by silica gel chromatography and the other was purified by EA extraction followed by silica gel chromatography. In the latter case, the residual PE was almost completely removed, whereas, in the former case, the residual PE was remained remarkably. Additionally, the purification yield of PE-gal was about 21% on the basis of mole. In the same purification protocol, CPN-gal was able to be purified using EA extraction followed by silica gel chromatography, in which the residual CPN was almost removed when CPN-gal was purified by EA extraction followed by silica gel chromatography.

• Analytical Science and Technology
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• v.23 no.6
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• pp.551-559
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• 2010

This study was conducted to establish an analytical method for the determination of seven nitrosamines in chlorinated tap water by precolumn derivatization followed by high performance liquid chromatography coupled with fluorescence detection. The derivatization procedure was optimized for denitrosation and dansylation, and then two extraction methods, liquid-liquid extraction (LLE) with dichloromethane and solid phase extraction (SPE), were compared. The SPE method employing the optimized derivation procedure showed higher extraction recovery (54.4-88.7%) and reproducibility (1.9-19.4%) than the LLE method (51.4-87.7% and 4.2-33.3%, respectively). The method detection limits were between 0.5 and 4.4 ng/L. When chlorinated water samples were collected from two treatment plants and ten household taps, and analyzed for nitrosamines, Nnitrosodimethylamine (NDMA) was the major compound found between 26.1 and 112 ng/L.