• Korean Journal of Environmental Agriculture
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• v.28 no.4
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• pp.427-434
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• 2009

Analytical method for prochloraz in cabbage, apple, pepper, mandarin, and hulled rice was established by conversion it to 2,4,6-trichlorophenol (TCP). Crop samples were extracted with acetonitrile, and partitioned with dichloromethane. The sample extracts were hydrolyzed with pyridine hydrochloride in a vial by heating for 1 hour, and analyzed with GC-ECD after partitioning with dichloromethane. Method quantification limit (MQL) of prochloraz was 0.01 mg/kg. Recoveries at 0.1 mg/kg level was 105-113% while at 0.5 mg/kg level was 82-87%. In both of the cases CV was less than 10%. Through this procedure soxhlet extraction and refluxing apparatus of conventional method were discarded and simple solvent extraction and small vial were successfully employed, resulting in simple, rapid, economic and more precise method.

• Proceedings of the PSK Conference
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• 2003.10b
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• pp.223.2-223.2
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• 2003

A rapid, sensitive and selective liquid chromatography-tandem mass spectrometric (LC/MS/MS) method for the determination of eupatilin in human plasma was developed. Eupatilin and internal standard, (S)-[N-3-(4-(2-(1-methyl-5-tetrazolyl)-pyridine-5-y1)- 3-fluorophenyl)-2-oxo-5-oxazolidinyl]methyl acetamide (DA-7867) were extracted from human plasma by liquid-liquid extraction and analyzed on a phenyl-hexyl column with the mobile phase of acetonitrile-ammonium formate (10 mM, pH 3.0) (60:40, v/v). (omitted)

• Journal of Conservation Science
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• v.32 no.3
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• pp.385-394
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• 2016

A fabric excavated from tombs or passed down is not easy to find its original color as it degrades and discolors by UV and visible rays, oxygen and microorganisms. LC-MS analysis is commonly used for separating and analyzing colors, but color extraction process is complicated and important in dye-qualitative analysis. To extract red colors from a fabric which is dyed with safflower and lac, solvents; hydrogen chloride, pyridine and oxalic acid are used and oxalic acid was the most effective solvent. Meanwhile, dyed samples were put in degradation condition; UV-A for 168 hours and analyzed with LC-MS to find out its colors'chemical changes. As a result, carthamin is detected in $T_R$ 13 min and laccaic acid A is detected in $T_R$ 10 min. However carthamin is not detected in a degraded fabric dying with safflower, it could be identified as a safflower fabric by the molecular weight of m/z 931. Through this study the most optimal method for red color extraction is found so it is expected to be used as a base line data for red color LC-MS analysis.

• Applied Chemistry for Engineering
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• v.19 no.1
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• pp.105-110
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• 2008

The high-purity purification of 2,6-dimethylnaphthalene (2,6-DMN, 10.43 wt%) from the concentrate of DMN isomers recovered from light cycle oil (LCO) through distillation-extraction combination was examined by a crystallization operation. To select the most suitable crystallization solvent for purification of 2,6-DMN, several conventional solvents, which have been employed commercially as crystallization solvents for high-purity performance, were tested, through measurement of purity and yield of 2,6-DMN. The solvents used were acetone, cyclohexanone, ethanol, ethyl ether, ethyl acetate, isopropyl ether, methanol, n-hexane, n-heptane, pyridine, THF, toluene, and a mixture of methanol and acetone. The mixture of 60 vol% methanol and 40 vol% acetone (M/A = 1.5) was found to be suitable for purification of 2,6-DMN in the concentrate of DMN isomers based on purity and yield. Increasing the operation temperature and the volume ratio of solvent (M/A = 1.5) to feed (concentrate of DMN) resulted in improving the purity of 2,6-DMN, whereas the yield decreased. The crystal recovered by crystallization run using the concentrate of DMN isomers contained about 76 wt% 2,6-DMN. Furthermore, for recovery of high-purity 2,6-DMN, crystal containing 76 wt% 2,6-DMN was crystallized. As a result, crystal with 99.7 wt% 2,6-DMN was recovered with 40% yield.

• Korean Journal of Food Science and Technology
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• v.36 no.4
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• pp.553-557
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• 2004

Aroma compounds in Pholiota adiposa were extracted by simultaneous distillation and extraction (SDE), and 41 compounds were identified by GC-MS, including eleven alcohols, eight aldehydes, four esters, four ketones, nine alkans, and five miscellaneous compounds. Major aroma compounds included hexanal (8.55%), n-heptaldehyde (13.02%), 2-pentyl furan (4.82%), benzeneacetaldehyde (3.34%), (E,Z)-2,4-decadienal (3.06%), and hexacosane(5.04%). Drying method was applied to aroma compounds of Pholiota adiposa extracted by solid phase microextraction and identified by GC-MS. As hot air-drying temperature increased, peak areas (%) of 2-phenylethanol and benzeneacetaldehyde decreased, whereas those of 2(5H)-furanone (0.16%), 2H-1-benzopyran-2-one (7.63%), 2-acetylpyrrole (5.49%), and 4-phenyl-pyridine (5.61%) increased significantly at $70^{\circ}C$.

• Journal of the Korean Society of Food Science and Nutrition
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• v.34 no.4
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• pp.513-518
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• 2005

Volatile compounds of $\gamma-irradiation$ leeks (Aillum tuberosum R.) were isolated by simultaneous steam distillation and extraction method (SDE) and analyzed by gas chromatography/mass spectrometry (GC/MS) along with the non-irradiated sample. Leeks were irradiated at dose of 20 kGy and non-irradiated samples were considered as control sample. 56 and 54 compounds were identified in non-irradiated and irradiated samples, respectively. These components included the functional groups; alcohols, aldehydes, esters, ketones, N- and S-containing compounds. S-containing compounds such as dimethyl trisulfide, methyl-(Z)-l-proenyl trisulfide, dimethyl disulfide, 3-ethyl-l,2-dithi-5-ene and methyl allyl disulfide were the major compounds. Methyl-(Z)-l-propenyl trisulfide, diallyl trisulfide, (E)-2-hexanal and 3-ethyl-l,2-dithi-5-ene were clearly decreased by the $\gamma-irradiation$, but dimethyl disulfide, diallyl sulfide, allyl methyl sulfide and pyridine were increased by the $\gamma-irradiation$.

• Journal of the Korean Chemical Society
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• v.30 no.4
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• pp.369-376
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• 1986

Diosgenin in an Indonesian Costus speciosus was determined by capillary gas-liquid chromatography (GLC). The experimental conditions for the hydrolysis, extraction and acetylation of the diosgenin, and the determination by GLC were investigated. 0.20g of dried sample powder was refluxed in the solution of 3N HCI and xylene at 95∼100${\circ}C$ for 4 hours and the xylene layer was separated. The residue evaporated the xylene was refluxed in 20 : 80 acetic anhydride-pyridine for 30 minutes and the diosgenin acetate was extracted with diethyl ether. Dehydrated with anhydrous $Na_2SO_4$ and evaporated the ether, the residue was dissolved in 5.00ml of n-hexane and injected into GLC. Capillary column of SE-30 25m ${\times}$ 0. 33mm was installed in GLC and the column temperature was increased from 180${\circ}$ to 270${\circ}C$ at rate of 10${\circ}C$/min. The flow rate of carrier gas $N_2$ was 2ml/min and FID was used to detect. The analytical result of the diosgenin was 0.281% and relative standard deviation of 5 measures was 1.8%.

• Analytical Science and Technology
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• v.6 no.1
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• pp.29-37
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• 1993

Some new podands containing phenyl(B), benzyl(Bz), pyridine(Py), quinoline(Q) and naphthalene(Np) as end-groups, and oxygen(O) and sulfur(S) in ether chains as donor atoms have been synthesized. The univalent cation binding characteristics of these podands have been studied by NMR titration and solvent extraction. By NMR titration we have found that the most of podands form 1:1 complexes with $Ag^+$ ion. Especially, the substituted sulfur atoms in ether chains show the effects to enhance the stabilities. We also carried out the extractions of univalent cation picrates including alkaline metal, $Ag^+$, $Tl^+$ and $NH_4{^-}$ ions from aqueous to chloroform layer by using these podands. We found that the extractabilities of $Ag^+$ ion with the quinoline-containing podands such as, $Q_2O_4$, $Q_2O_5$ and $BQO_5$ were 86.8, 86.6 and 48.0% respectively, but the naphthalene-containing podands such as, $Np_2O_4$ and $Np_2O_5$ extracted quite small amount. Otherwise, in cases of $Bz_2O_3S_2$(89.4%), $B_2O_2S_2$(96.8%), $B_2O_3S_2$(58.9%), $Py_2O_2S_2$(58.8%), $Py_2O_3S_2$(42.1%), and $B_2O_4S$(15.0%), interestingly, $Bz_2O_3S_2$ which have sulfur atoms and benzyl groups showed the highest extraction selectivity for $Ag^+$ ion. This result seems due to not only the strong interaction of $Ag^+$ ion with sulfur donors according to the HSAB theory, but also the effective ${\pi}-{\pi}$ stacking interaction between two aromatic end-groups which is enhanced by the flexible methylene spacing group in benzyl groups instead of phenyl groups. The extraction coefficients gave the similar tendency as the extractabilities and the stabilities. From these results, it could be concluded that the predominant factor affected to extraction coefficients is the stabilities, which are strongly influenced by the structures of podands.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.48 no.5
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• pp.668-673
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• 2015

The pacific oyster Crassostrea gigas has a desirable taste and flavor that differs from those of other fish and shellfish. In order to develop a high value-added product from individually quick-frozen oyster extract (IQFOE), we prepared an oyster sauce from IQFOE and characterized its volatile compounds using vacuum simultaneous steam distillationsolvent extraction / gas chromatography / mass spectrometry. The moisture, crude protein, crude ash, salinity, pH and volatile basic nitrogen contents of the oyster sauce were 60.6%, 8.2%, 9.2%, 9.3%, 5.7 and 21.0 mg/100 g, respectively. Seventy-six volatile compounds were detected in the cooked odor of the oyster sauce. These volatile compounds included 14 esters, including ethyl acetate, 13 nitrogen- containing compounds, including 2,4,6-trimethyl pyridine, 13 acids, including hexadecanoic acid, 12 alcohols, including ethyl alcohol and 6-methyl heptanol, 6 alkanes, 5 aldehydes, including benzaldehyde, 5 ketones, including 1-(2-furanyl)-ethanone, 4 furans, including 2-furancarboxaldehyde and 2-furanmethanol, 3 aromatic compounds, including d-limonene, and 1 miscellaneous compound. Esters, acids and nitrogen-containing compounds, and alcohols were the most abundant compounds in the odor of the cooked oyster sauce, with some aldehydes, ketones, and furans.

• Journal of Food Hygiene and Safety
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• v.13 no.2
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• pp.129-134
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• 1998

To develop an enzyme-linked immunosorbent assay (ELISA) for nivalenol (NIV), we produced polyclonal antibodies against tetraacetyl nivalenol (Ac4-NIV) and established ELISA conditions. Ac4-NIV-hemisuccinate conjugated to bovine serum albumin (Ac4-NIV-HS-BSA) was immunized with Freund's adjuvants into rabbits subcutaneously several times. By use of the antiserum showing the highest titer and Ac4-NIV-HS-HRP conjugate, we established competitive direct ELISA (cdELISA). Standard curve of cdELISA showed that the detection range of Ac4-NIV was about 10~5,000 ng/ml (ppb). The cross-reactivities of the polyclonal antibody towards Ac4-NIV and acetyl T-2 were 100 and 70% respectively, and those towards NIV, deoxynivalenol, 3-acetyl deoxynivalenol, 15-acetyl deoxynivalenol, triacetyl deoxynivalenol, fusarenonX, and T-2 were less than 0.1%. When cdELISA was applied to NIV-spiked corns followed by extraction with 70% acetonitrile and acetylation with acetic anhydride in pyridine, the recovery rates of the Ac4-NIV were 108, 143, and 70% (average, 107%) in the levels of 100, 300, and 1,000 ng/g (ppb), respectively.