• Journal of fish pathology
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• v.34 no.2
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• pp.261-269
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• 2021

This study presents the evaluation of sample extraction and purification procedure for the determination of residues of febantel and its metabolites, fenbendazole, oxfendazole and oxfendazole sulfone in rockfish (Sebastes schlegeli) muscle using liquid chromatography-tandem mass spectrometry. Residues of febantel and its metabolites in rockfish muscle were analyzed using each different sample preparation method from Korean Food Standards Codex (KFSC), Food Safety and Inspection Service (FSIS, USA), and the modified FSIS method using QuEChERS kit (FSIS-Q), respectively. Each method was compared for mean recoveries and repeatabilities. Since FSIS-Q showed higher repeatabilities (coefficient of variation, CV of 2.4%~10.9%) than those of FSIS method (CV of 4.6%~17.5%), recoveries from FSIS-Q were compared with those from KFSC method. FSIS-Q showed significantly higher recoveries of 83.1%~110.1% (P < 0.05) than those from KFSC method of 64.7%~107.4%. In addition, FSIS-Q showed a good linearity over the range of 2.5~200 ㎍/kg, and excellent sensitivities with limit of detection of 0.46~0.71 ㎍/kg and limit of quantification of 1.08~2.15 ㎍/kg. Although all the sample preparation methods turned out to be able to meet CODEX guideline for all the compounds, FSIS method and FSIS-Q validated in this study could be applied to screening and quantification for residues of febantel and its metabolites in rockfish muscle with efficient preparation procedures.

• Bulletin of the Korean Chemical Society
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• v.13 no.2
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• pp.199-207
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• 1992

The approximate rates and stoichiometry of the reaction of excess sodium diethyldihydroaluminate (SDDA) with 68 selected organic compounds containing representative functional groups were examined under standard conditions (THF-toluene, $0^{\circ}C$ in order to compare its reducing characteristics with lithium aluminum hydride (LAH), aluminum hydride, and diisobutylaluminum hydride (DIBAH) previously examined, and enlarge the scope of its applicability as a reducing agent. Alcohols, phenol, thiols and amines evolve hydrogen rapidly and quantitatively. Aldehydes and ketones of diverse structure are reduced rapidly to the corresponding alcohols. Reduction of norcamphor gives 11% exo-and 89% endo-norborneol. Conjugated aldehydes such as cinnamaldehyde are rapidly and cleanly reduced to the corresponding allylic alcohols. p-Benzoquinone is mainly reduced to hydroquinone. Hexanoic acid and benzoic acid liberate hydrogen rapidly and quantitatively, however reduction proceeds very slowly. Acid chlorides and esters tested are all reduced rapidly to the corresponding alcohols. However cyclic acid anhydrides such as succinic anhydride are reduced to the lactone stage rapidly, but very slowly thereafter. Although alkyl chlorides are reduced very slowly alkyl bromides, alkyl iodides and epoxides are reduced rapidly with an uptake of 1 equiv of hydride. Styrene oxide is reduced to give 1-phenylethanol quantitatively. Primary amides are reduced very slowly; however, tertiary amides take up 1 equiv of hydride rapidly. Tertiary amides could be reduced to the corresponding aldehydes in very good yield ( > 90%) by reacting with equimolar SDDA at room temperature. Hexanenitrile is reduced moderately accompanying 0.6 equiv of hydrogen evolution, however the reduction of benzonitrile proceeds rapidly to the imine stage and very slowly thereafter. Benzonitrile was reduced to give 90% yield of benzaldehyde by reaction with 1.1 equiv of hydride. Nitro compounds, azobenzene and azoxybenzene are reduced moderately at $0^{\circ}C$, but nitrobenzene is rapidly reduced to hydrazobenzene stage at room temperature. Cyclohexanone oxime is reduced to the hydroxylamine stage in 12 h and no further reaction is apparent. Pyridine is reduced sluggishly at $0^{\circ}C$, but moderately at room temperature to 1,2-dihydropyridine stage in 6 h; however further reaction is very slow. Disulfides and sulfoxides are reduced rapidly, whereas sulfide, sulfone, sulfonic acid and sulfonate are inert under these reaction conditions.

• Food Science of Animal Resources
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• v.41 no.1
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• pp.59-70
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• 2021

A method for simultaneous detection of fipronil (F) and its metabolites fipronil desulfinyl (FD), fipronil sulfide (FS), fipronil sulfone (FSO) in chicken eggs was applied and validated. It includes single-step, cheap, effective, rugged, safe-based method (SinChERS) for sample preparation and ultra high performance liquid chromatography coupled with mass spectrometry (UHPLC-MS/MS) for chemical analysis. Results suggested that formic acid enhanced the recovery of 4 target residues and 1% supplementation to acetonitrile gained higher recoveries than that of 5%. SinChERS integrated extraction and clean-up steps into one, with shorter time (1.5 h) to operate and higher recoveries (97%-100%) than HLB, Envi-Carb-NH2 and quik-easy-cheap-effective-rugged-safe method (QuEChERS), and it consumed the smallest volume of extracting solvent (10 mL) as QuEChERS. Quantitative analyses using external standard method suggested the linear ranges of 4 target compounds were 1-20 ㎍/L with R2 >0.9947. The limit of detection (S/N>3) and quantification (S/N>10) were 0.3 ㎍/kg and 1 ㎍/kg. Recoveries ranged from 89.0% to 104.4%, and the relative standard deviations (n=6) at 1, 10, and 20 ㎍/kg were lower than 6.03%. Thirty batches of domestic eggs (500 g each) were detected by the established SinChERS-based UHPLC-MS/MS and no target residues were detected in all samples. The method developed in this study is a rapid, sensitive, accurate and economic way for multi-residue analysis of fipronil and its metabolites in eggs.

• Transactions of the Korean hydrogen and new energy society
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• v.33 no.3
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• pp.209-218
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• 2022

Recently, research on the development of anion exchange membranes (AEMs) has received considerable attention from the scientific community around the world. Here, we fabricated a series of AEMs with branched structures with different alkyl spacers and conducted comparative evaluations. The introduction of these branched structures is an attempt to overcome the low ionic conductivity and stability problems that AEMs are currently facing. To this end, branched polymers with different spacer lengths were synthesized and properties of each membrane prepared according to the branched structure were compared. The chemical structure of the polymer was investigated by proton nuclear magnetic resonance, Fourier transform infrared, and gel permeation chromatography, and the thermal properties were investigated using thermogravimetric analysis. The branched anion exchange membrane with (CH₂)₃ and (CH₂)₆ spacers exhibited ionic conductivities of 8.9 mS cm^-1 and 22 mS cm^-1 at 90℃, respectively. This means that the length of the spacer affects the ionic conductivity. Therefore, this study showing the effect of the spacer length on the ionic conductivity of the membrane in the polymer structure constituting the ion exchange membrane is judged to be very useful for future application studies of AEM fuel cells.

• Food Science of Animal Resources
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• v.43 no.5
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• pp.914-937
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• 2023

The objective of this study was to establish a multi-residue quantitative method for the analysis of anthelmintic and antiprotozoal drugs in various livestock products (beef, pork, and chicken) using ultra-high-performance liquid chromatography-tandem mass spectrometry. Each compound performed validation at three different levels i.e., 0.5, 1, and 2× the maximum residue limit according to the CODEX guidelines (CAC/GL 71-2009). This study was conducted according to the modified quick, easy, cheap, effective, rugged, and safe procedure. The matrix-matched calibrations gave correlation coefficients >0.98, and the obtained recoveries were in the range of 60.2%-119.9%, with coefficients of variation ≤32.0%. Furthermore, the detection and quantification limits of the method were in the ranges of 0.03-3.2 and 0.1-9.7 ㎍/kg, respectively. Moreover, a survey of residual anthelmintic and antiprotozoal drugs was also carried out in 30 samples of beef, pork, and chicken collected in Korea. Toltrazuril sulfone was detected in all three samples. Thus, our results indicated that the developed method is suitable for determining the anthelmintic and antiprotozoal drug contents in livestock products.

• Membrane Journal
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• v.32 no.1
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• pp.13-22
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• 2022

Ever increasing global energy demand gives rise to uncontrollable environmental pollution. Demand on fossil fuel and consequent carbon emission leads to global warming and climate change. Nuclear energy is an alternative source to generate clean energy but mining of nuclear fuel is associated with harmful chemicals. Mining of valuable minerals from sea water by membrane separation process is a cost effective along with environmental friendly process. Separation and adsorption based mining of valuable minerals from sea water are another efficient process. Recovery of actinides from rare earth elements are very challenging and expensive process. Pressure driven membrane separation process is economically more viable along with environmental process. In this review membrane separation process are based on polyether sulfone, polyamide, polyimide, polyamidoxine and hybrid membranes. In case of adsorption process, mainly amidoxime kind of adsorbent are discussed.

• Composites Research
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• v.12 no.4
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• pp.71-78
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• 1999

To determine the effect of chemical structure of linear amine curing agents on thermal and mechanical properties, standard epoxy resin DGEBA was cured with diaminodiphenyl methane (DDM), diaminodiphenyl sulphone (DDS) in a stoichiometrically equivalent ratio. From this work, the effect of aromatic amine curing agents. In contrast, the results show that the DGEBA/DDS cure system having the sulfone structure between the benzene rings had higher values in the conversion of epoxide, density, shrinkage (%), glass transition temperature, tensile modulus and strength, flexural modulus and strength than the DGEBA/DDM cure system having methylene structure between the benzene rings, whereas the DGEBA/DDM cure system presented higher values in the maximum exothermic temperature, thermal expansion coefficient, and thermal stability. These results are caused by the relative effects of sulfone group having strong electronegativity and methylene group having (+) repulsive property and stem from the effect of the conversion ratio of epoxide group. The result of fractography shows that the each grain size of the DDM/DGEBA system with feather-like structure is larger than that of the DDS/DGEBA system.

• Journal of the Korean Chemical Society
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• v.37 no.3
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• pp.351-354
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• 1993

Z-1-Ethyl-2-nitro-l-butenyl-(4'-methyl)-phenyl sulfone, C$_{13}$H$_{17}$NO$_4$S, Mr = 293.4, monoclinic space group P2$_1$/c, a = 12.194(7), b = 7.290(4), c = 16.532(14)${\AA}$, ${\beta}$ = 103.4(2)$^{\circ}$, V = 1429.5 ${\AA}^3$, Z = 4, D$_c$ = 1.32 gcm$^{-3}$, ${\lambda}$(Mo K${\alpha}$) = 0.71069 ${\AA}$, ${\mu}$ = 2.2 cm$^{-1}$, F(000) = 600, T = 298 K, R = 0.030 for 1762 unique observed reflections with I > 1.0${\sigma}$(I). A molecule has a cis-typed molecular structure having the form of "the substituted butene backbone, C-C(S)=C(NO$_2$)-C, connecting to a sulfur atom with the methylbenzene ring and to a nitro group. The methylbenzene ring and the substituted butene moiety are nearly planar with the maximum deviations from their own molecular planes, 0.018 ${\AA}$ for the C(1) atom of the benzene group and 0.045 ${\AA}$ for the N atom of the NO$_2$ group, respectively. The angles to the plane of the butene backbone are 88.5$^{\circ}$from the plane of the methyl-benzene and 78.6$^{\circ}$from the plane of the nitro group. Rotation of the nitro group from the butene plane seems to reduced contribution of resonance structure involving the nitro group, and resultant repulsion between the O(2) atom of SO$_2$ and the O(3) atom of NO$_2$ appears to be 2.894 ${\AA}$ longer than an expected van der Waals distance of 2.80 ${\AA}$.

• Journal of Food Hygiene and Safety
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• v.30 no.3
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• pp.272-280
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• 2015

A simultaneous official method was developed for the determination of phorate and its metabolites (phorate sulfoxide, phorate sulfone, phorate oxon, phorate oxon sulfoxide, phorate oxon sulfone) in livestock samples. The analytes were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Phorate and its metabolites were extracted from beef and milk samples with acidified acetonitrile (containing 1% acetic acid) and partitioned with anhydrous magnesium sulfate. Then, the extract was purified through primary secondary amine (PSA) and C18 dispersive sorbent. Matrix matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/L) for all the analytes into blank extract with $r^2$ > 0.996. For validation purposes, recovery studies were carried out at three different concentration levels (beef 0.004, 0.04 and 0.2 mg/kg; milk 0.008, 0.04 and 0.2 mg/kg, n = 5). The recoveries were within 79.2-113.9% with relative standard deviations (RSDs) less than 19.2% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines. The limit of quantification was quite lower than the maximum residue limit (MRL) set by the Ministry of Food and Drug Safety (0.05 mg/kg). The proposed analytical method was accurate, effective and sensitive for phorate and its metabolites determination and it will be used to as an official analytical method in Korea.

• Korean Journal of Soil Science and Fertilizer
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• v.24 no.2
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• pp.116-123
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• 1991

Two solution to soil ratios, 2 : 1 and 5 : 1 were tested to determine the appropriate ratio in the sorption measurement off. sulfoxide for Wahiawa soil samples, 0-20 cm, 40-60 cm and 100-120 cm. and Salinas soil samples, 0-15cm and 115-130cm. One ${\mu}$ mol/L f.sulfoxide was used as an initial equilibration concentration. Sorption of f.sulfoxide at 5 : 1 ratio showed appropriate mixing, while sorption at 2 : 1 ratio indicated insufficient mixing during the various batch equilibration times (4, 12, 24 and 48 hours). For most samples the degree of sorption was about 20-50%, which falls in the desired range (20-80%) at the 5 : 1 ratio. An exception was with the low-sorptive Wahiawa subsoil in which the ranges were below 20%. Thus the 5 : 1 ratio can be used for f.sulfoxide sorption measurement. Four equilibration times (4, 12, 24 and 48 hours) and four concentrations(0.1, 1.0, 5.0 and $10{\mu}mol/L$) were used to determine the appropriate equilibration time for Wahiawa and Salinas soils. Sorption increased over all equilibration times, indicating no complete equilibrium within 48 hours. Apparent equilibrium was reached in 4 hours, and sorption increased slowly until 24 hours and faster thereafter, except for the Wahiawa soil, 100-120 cm. The recommended equilibration time is 24 hours, since it may eliminate the insufficient sorption and yet avoid undesirable transformation.