• Applied Biological Chemistry
• /
• v.41 no.8
• /
• pp.595-599
• /
• 1998

An analytical method was developed to determine tricyclazole residues in rice grain, straw, and soil using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. Tricyclazole was extracted with methanol from moist rice grain, straw, and soil samples. n-Hexane washing was employed to remove nonpolar co-extractives during liquid-liquid partition. Tricyclazole was then extracted with dichloromethane from alkaline aqueous phase, while acidic interferences remained in the phase. Dichloromethane extract was further purified by silica gel column chromatography prior to HPLC determination. Reverse-phase HPLC using an octadecylsilyl column was successfully applied to separate and quantitate the tricyclazole residue in sample extracts monitored at ${\lambda}_{max}$ 225nm. Recoveries from fortified samples averaged $95.5{\pm}3.0%\;(n=6),\;87.5{\pm}20.%\;(n=6),\;and\;84.3{\pm}2.8%$ (n=12) for rice grain, straw, and soil, respectively. Detection limit of the method was 0.02 mg/kg for rice grain and soil samples while 0.05 mg/kg for rice straw samples. The proposed method was reproducible and sensitive enough to evaluate the safety of tricyclazole residues in rice grain, straw, and soil.

• Journal of the Korean Wood Science and Technology
• /
• v.24 no.3
• /
• pp.45-50
• /
• 1996

Wood chips of oak(Quercus mongolica) and larch(Larix leptolepis) were treated with low pressure steaming explosion. Main components of exploded wood were separated with hot water and methanol extraction. Crude lignin separated from those extractives were purified and those chemical characteristics were investigated. And also, lignin adhesive was prepared from crude lignin and studied those chemical characteristics. The results can be summarized as follows ; 1. The purified lignin by Bj$\ddot{o}$kman's method from crude lignin is about 30% in exploded oak wood and is about 11% in exploded larch wood as a low amount. 2. The phenolic hydroxyl groups in the purified lignins are little higher than those of MWL and molecular weight distributions of the purified lignins are some lower than that of MWL. 3. Alkaline nitrobenzene oxidation products are very low in the clude lignin but those are increased in the purified lignin 4. The gravity of lignin resins(1.15 and 1.13) are a little lower than that of phenol resin(1.16) and the compressive shearing strength of lignin resins are higher than those of phenol resin.

• Korean Journal of Environmental Agriculture
• /
• v.23 no.4
• /
• pp.251-257
• /
• 2004

Analytical methods were developed to determine cyclosulfamuron residues in soil, water, rice grain and straw using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. In these methods, cyclosulfamuron was extracted with aqueous $Na_2HPO_4$/acetone and acetone/methanol mixture from soil and rice samples respectively. Liquid-liquid partition coupled with ion-associated technique, Florisil column chromatography, and solid-phase extraction (SPE) were used to separate cyclosulfamuron from interfering co-extractives prior to HPLC analysis. For water sample, the residue was enriched in $C_{18}$-SPE cartridge, cleaned up in situ, and directly subjected to HPLC. Reverse-phase HPLC under ion-suppression was successfully applied to determine cyclo-sulfamuron in sample extracts with the detection at its ${\lambda}_{max}$ (254 nm). Recoveries from fortified samples averaged $87.8{\pm}7.1%$ (n=12), $97.3{\pm}7.2%$ (n=12), $90.8{\pm}6.6%$ (n=6), and $78.5{\pm}6.7%$ (n=6) for soil, water, rice grain and straw, respectively. Detection limits of the methods were 0.004 mg/kg, 0.001 mg/L, 0.01 mg/kg and 0.02 mg/kg for soil, water, rice grain and straw samples, respectively.

• Journal of the Korean Wood Science and Technology
• /
• v.31 no.2
• /
• pp.45-51
• /
• 2003

One flavonoid, lignan glycosides and two diarylheptanoids were isolated from the sapwood of Betula maximowicziana. The structures were determined as : catechin 7-O-𝛽-D-xylopyranoside, lyoniresinol 9'-O-𝛽-D-glucopyranoside, 11-oxo-3, 8, 12, 17-tetrahydroxy-9-ene[7, 0]-metacyclophane and 11-oxo-3, 8, 9, 10, 12, 17-hexahydroxy[7, 0]-metacyclophane, respectively, on the basis of spectrosopic data and chemical correlations.

• Journal of the Korean Wood Science and Technology
• /
• v.34 no.3
• /
• pp.73-83
• /
• 2006

The dried needles (1.5 kg) of Abies koreana and Abies holophylla were ground, extracted with acetone-$H_2O$ (7:3, v/v), concentrated, and fractionated with a series of hexane, methylene chloride, ethyl acetate and water on a separatory funnel. Each fraction was freeze dried, then a portion of ethyl acetate soluble powder was chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-hexane mixture as eluents. The isolated compounds were identified by cellulose TLC, $^1H$, $^{13}C-NMR$, COSY, HETCOR, FAB and EI-MS. The needles of Abies koreana and Abies holophylla contained a large amount of aromadendrin-7-O-${\beta}$-D-glucopyranoside (compound III), polydatin (compound VI), (-)-rhododendrol-2-O-${\beta}$-D-glucopyranoside (compound VII), in addition to a small amount of (+)-catechin (compound I), kaempferol-3-O-${\beta}$-D-glucopyranoside (compound IV), myricetin-3-O-${\beta}$-D-glucopyranoside (compound V), naringenin-7-O-${\beta}$-D-glucopyranoside (compound II). DPPH analysis was also tested to investigate the antioxidative effects on the isolated compounds and (+)-catechin and polydatin were effective.

• Applied Biological Chemistry
• /
• v.39 no.4
• /
• pp.327-331
• /
• 1996

This experiment was conducted to establish the efficient extraction condition for anthocyanin and tannin pigments contained in rice bran of colored rices. Efficiency of the pigment extraction was maximum when the concentration of mired solvent of methanol(3) : ethanol(7) was 70%. In purple rite(anthocyanin pigment), ‘Kilimheugmi’, 80% ethanol containing 0.5% malic acid showed the highest extraction efficiency and stability with a maximum absorbance wavelength$(\lambda_{max})$ at 538 nm. In red rice(tannin pigment), ‘Jagwangdo’, 80% ethanol containing 0.01% citric acid showed the highest extraction efficiency and stability with a maximum absorbance wavelength$(\lambda_{max})$ at 456 nm. The relative optical density of the pigments increased until the solvent temperature was reached at $70^{\circ}C$, but drastically decreased over at $90^{\circ}C$ due to color change. The higher amount of the pigment was ertracted from the longer shaking time of the solvent. Ten minutes was enough for the grinding time of rite bran in solvent. Supernatant of the pigment extractives after one day storage at $4^{\circ}C$ in dark chamber revealed higher optical density than the filtration of the pigment extractives.

• Journal of the Korean Wood Science and Technology
• /
• v.30 no.1
• /
• pp.63-71
• /
• 2002

The bark of P. alba × glandulosa, P. euramericana and P. nigra × maximounczii F₁, several Populus trees, were collected, extracted with acetone-H₂O(7:3, v/v), fractionated with hexane, chloroform and ethylacetate, and freeze dried to give some dark brown powder. Each fraction of the powder was chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-hexane mixture as eluents and then identified by thin layer chromatography using TBA and 6% acetic acid as developing solvents. The structures of the isolated compounds were characterized by ¹H, ¹³C and 2D-NMR tools including mass spectrometry. Most of the compounds were flavonoids and salicin derivatives as follows: (+)-catechin, taxifolin, aromadendrin, eriodictyol, naringenin, sakuranetin, sakuranetin-5-O-𝛽-D-glucopyranoside, neosaturanin, salireposide, p-coumaric acid, and aesculin from P. alba × glandulosa, (+)-catechin, salireposide, populoside and salicortin from P. euramericana and (+)-catechin, quercetin, padmatin, salireposide, populoside and salicortin from P. nigra × maximounczii F₁.

• Journal of the Korean Society of Tobacco Science
• /
• v.14 no.2
• /
• pp.159-167
• /
• 1992

It would be clear that the constituents of the leaf surface lipid is ye비 important as an evaluation index of tobacco leaf quality since the quality of tobacco specific aroma with leaf species depends on the contents of the lipid and the strength of the aroma is determined by the amounts of the lipid secreted. For the reason, a rapid and peproducible method to quantify DVT, which is a kind of lipid, has been studied. The biosynthesis procedure of DVT in leaf growing processes, and the volatile or decompositional characters of DVT in leaf drying processes were also discussed. In consequence, it might be possible to get the data available to the cultivation of better tobacco leaf and the manufacture of cigarettes with better aroma and taste. The results obtained from this study are as follows. 1. Chloroform/dichloromethane solvent was better than chloroform alone for DVT extraction. The extraction yields of the leaf surface lipid were about 5% 2. The extractives with dichloromethane were treated by silylation with BSTPa and the quantitative analysis of DVT was carried out using SE -54 fused silica capillary column. It was found that rapid and reproducible data could be obtained from these methods. 3. In flue - cured tobacco species, DVT contents were $30.3\mu\textrm{g}/cm^2$ in the beginning stage of leaf drying processes and $12.1\mu\textrm{g}/cm^2$ corresponded to 30% levels of the beginning stage, in the end stage. 4. DVT contents in Burley mere 2 times as large as those in fluecured tobacco. DVT in the upper stalk position of leaf was 3 times larger than that in the lower stalk position. 5. DVT of tobacco leaves was decomposed by $SO_2$ gas or the sun light. The decomposition rate was largest in the sample used methanol as a extraction solvent.

• Journal of Forest and Environmental Science
• /
• v.18 no.1
• /
• pp.53-60
• /
• 2001

2kg of the dried leaves of chamaecyparis obtusa Endlicher were ground, extracted with acetone-$H_2O$(7:3, v/v), concentrated, and fractionated with a series of hexane, $CH_2Cl_2$, EtOAc and water on a separatory funnel. Each fraction was freeze dried to give dark-brown powder and a EtOAc soluble portion of the powder was chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-hexane mixture as eluents. Spectrometric analyses such as NMR and FAB-MS including TLC were performed to characterize the structures of the isolated compounds. The leaves of chamaecyparis obtusa Endlicher contained a large amount of taxifolin-3-O-${\beta}$-D-xylopyranoside and (+)-catechin in addition to a small amount of quercetin-3-O-${\alpha}$-L-rhamnopyranoside.

• Journal of the Korean Wood Science and Technology
• /
• v.34 no.1
• /
• pp.79-85
• /
• 2006

Paulownia coreana Uyeki fruits were collected, extracted with acetone-$H_2O$ (7:3, v /v), fractionated with n-hexane, methylene chloride, and ethyl acetate, then freeze dried to give some dark brown powder. The ethyl acetate soluble mixture was chromatographed on a Sephadex LH-20 column using a series of aqueous methanol and ethanol-hexane mixture as eluents. Spectrometric analysis such as NMR and MS including TLC were performed to establish the structures of the isolated compounds. From the ethyl acetate fraction, one phenolic acid (I) and five flavonoids (II~VI) and were isolated and elucidated. The antioxidative activities were tested on the isolated compounds, crude and fractionated extractives by DPPH radical scavenging method. The result showed that caffeic acid, kaempferol, luteolin, quercetin and the EtOAc soluble fraction exhibited higher activities than those of ${\alpha}$-tocopherol and BHT.