• Applied Biological Chemistry
• /
• v.40 no.5
• /
• pp.442-446
• /
• 1997

A new analytical method was developed by HPLC after supercritical fluid extraction and fluorogenic derivatization for the determination of quinclorac (3,7-dichloro-8-quinoline carboxylic acid) in soil. The graminicide quinclorac was extracted from soil by supercritical fluid extraction. Supercritical carbon dioxide at 7000 psi $(80^{\circ}C)$ modified with 30% of methanol extracted quinclorac from soil samples at the level of $0.1ng\;g^{-1}$ with 96% recovery. Extracted quinclorac was determined by HPLC as a fluorescent derivative. Derivatization was made with 4-bromomethyl-7-methoxycoumarin (4-Br-Mmc) using 18-crown-6-ether as a catalyst. The conversion was completed within 30 min and the limit of detection was 0.5 ppb to prove that the procedure could be used in the residue analysis of the pesticides containing carboxylic acid group.

• KSBB Journal
• /
• v.14 no.1
• /
• pp.17-23
• /
• 1999

Studies were carried out to elucidate the effects of pressure, temperature and mobile phase composition on supercritical $CO_2$ chromatographic separations of paclitaxel, baccatin III, 10-deacetyl baccatin III, 7-epi-10-deacetyltaxol, cephalomanine, and 10-deacetyltaxol. High resolutions of paclitaxel, 10-deacetylbaccatin III, 10-deacetyltaxol were observed with optimized pressure, temperature, and mobile phase composition. The highest resolution between paclitaxel and 10-deacetylbaccain III was observed at 275 kg/$\textrm{cm}^2$, $40^{\circ}C$ with the mobile phase composition of gradient mixture of 3.9-3.6 mL/min $CO_2$, 0.1-0.4 mL/min methanol for 20 min. Resolutions of baccatin III, capalomannine, and 7-epi-10-deacetyltaxol were found to be low in this study. On-line coupled SFE/SFC process was applied to isolate paclitaxel from yew tree powder. As a consequence, paclitaxel with a purity of 95% was obtained with a recovery yield of 38%.

• KSBB Journal
• /
• v.14 no.4
• /
• pp.408-413
• /
• 1999

To separate mixtures analytically and preparatively by LC (Liquid Chormatography), the operating conditions of analytical chromatography should be determined. The HCI program was utilized to find the optimum operating condition accurately and rapidly, and to reduce the number of experiments. In an analytical chromatography, based on the resolution and analysis time, the experimental conditons of deoxyribonucleosides and phopholipids were fixed in terms of taxol was calculated, and the collection time was predicted for the mixture of 5'-IMP and 5'-GMP from the elution profile when and purity wer known.

• Korean Journal of Food Science and Technology
• /
• v.31 no.5
• /
• pp.1268-1274
• /
• 1999

Pine twigs with buds were cut into $2{\sim}3\;mm$ long pieces and about 18g was used for each experiment. Pressure and temperature ranges employed were $100{\sim}300\;bar$ and $35{\sim}55^{\circ}C$, respectively. Volatile compounds of extracts were isolated and identified by gas chromatography and mass selective detector. Twenty three compounds from the extracts were identified. Limonene and ${\beta}-pinene$ were found to be the major components with $32.6{\sim}43.4%$ being limonene. Extracts obtained by supercritical fluid extraction were lower in monoterpene and higher in oxygenated terpenoids than those by steam distillation and solvent extraction (SDE). Sensory evaluation showed that the pine flavor extracted using supercritical carbon dioxide was much better in quality than that of SDE. In conclusion, it was found out that supercritical fluid extraction can successfully be applied to extract high quality flavor from pine.

• Applied Biological Chemistry
• /
• v.44 no.3
• /
• pp.197-201
• /
• 2001

Extraction efficiency of ${\beta}-ecdysone$ in Achyranthis radix was investigated using the methods of solvent extraction and supercritical fluid extraction (SFE). The optimum SFE conditions for the analysis of ${\beta}-ecdysone$ in A. radix were 300 atm, $80^{\circ}C$, 100 ml of extraction volume, and 20% ratio of modifier(methanol). As revealed through SFE, detection limit of ${\beta}-ecdysone$ in A. radix was 5 ng and recoveries of ${\beta}-ecdysone$ in A. radix shoots and root were $90.7{\sim}93.5%$ and $77.8{\sim}81.9%$, respectively. Recoveries of ${\beta}-ecdysone$ in A. radix shoots and root through solvent extraction were $76.4{\sim}93.0%$ and $80.6{\sim}93.1%$, respectively. ${\beta}-Ecdysone$ content was determined to be highest at 654.9 ppm in the first year A. radix roots harvested in August.

• Korean Journal of Food Science and Technology
• /
• v.31 no.5
• /
• pp.1300-1307
• /
• 1999

Supercritical fluid extraction was applied to recycling triglyceride from used shortening. Used shortening and its fractions were analyzed with high performance size exclusion chromatography for their composition in triglycerides, polymer and low molecular weight compounds. Conjugated diene value and color of the fractions were also measured with a UV spectrophotometer and a colorimeter, respectively. Pressure and temperature ranges employed were $15{\sim}30$ MPa and $40{\sim}60^{\circ}C$, respectively. Concentration of fat in supercritical (SC) $CO_2$ ranged from $0.3\;X\;10^{-3}{\sim}7.4\;X10^{-3}(g\;fat/g\;CO_2)$. An exponential relation between concentration of fat in SC $CO_2$ and density was observed. Color of the extracts was light yellow which was very close to that of the fresh shortening. Low molecular weight compounds were preferentially concentrated in the initial fraction, while polymer was extracted in the final fraction. Conjugated diene value of the initial fractions was clearly lower than that of feed. It increased sharply as the polymer content in the fraction became significantly large.

• Korean Chemical Engineering Research
• /
• v.53 no.1
• /
• pp.53-56
• /
• 2015

In this study, investigated the synthesis method of p-Phenylenediamine (PPD) by amination of p-Diiodobenzene (PDIB) under supercritical ammonia and CuI catalyst conditions. We examined the effects of various process variables (e.g., reaction temperature, pressure, amount of ammonia inserted, amount of catalyst inserted, and reaction time) on the production yield of PPD by analyzing the Gas Chromatography (GC). The experimental results demonstrated that PPD was not produced under non-catalyst conditions, and PPD production yield increased with increasing temperature, pressure, amount of catalyst inserted, and reaction time. However, for the reaction temperature case, it was found that $200^{\circ}C$ was the optimal temperature, because thermal degradation of PPD occurred above $250^{\circ}C$. In addition, we confirmed the structure of PPD and the bonding characteristics of the amine group via FT-IR and H-NMR analysis.

• Korean Journal of Medicinal Crop Science
• /
• v.11 no.2
• /
• pp.115-121
• /
• 2003

Essential oils from Fennel fruit(Foeniculum vulgare Mill), Olibanum resin(Boswellia carteii Birew) and Needl Juniperus stem(Juniperus rigida Sieb.) were extracted by a supercritical fluid extraction system(SFE) and biological activity of each essential oils were observed. SFE technique was applied for the isolation and purification of nonpolar biologically active essential oils from each samples. The quantitative analysis of essential oils was carried out by gas chromatography-mass spectrometer(GC/MS). About 60% of the growth of AGS and A549 cells were inhibited by adding 1.0g/l of the crude essential oils and below 40% was observed by the control. Cytotoxicity on human normal lung cell(HEL299) was scored as $15{\sim}18%$ for the crude essential oils and 12% for control, respectively. It meant that the essential oils were more effective than the control in anti-mutagenecity tested by CHO V79 cells. The effect of the essential oils on the growth of nerve cells, PC12 was observed as follows: The viable cell density was about two times higher than control.

• Korean Journal of Fisheries and Aquatic Sciences
• /
• v.34 no.3
• /
• pp.213-217
• /
• 2001

In order to develop a new separation technology, supercritical fluid extraction process was used to produce high purity pigments and fatty acids from seaweed (Undaria pinnatifida). Supercritical carbon dioxide was used as a solvent and ethanol as an entrainer. The sample was treated by a frozen drier and experiments were conducted with a semi-batch flow system at various operating conditions (pressure range, $10.3\~17.2$ MPa; temperature range, $30\~45^{\circ}C$: particle size, $500\~1,000{\mu}m$ extraction time, 60 min). Characteristics of the recovered pigment (chlorophyll a) and fatty acids were determined by UV-spectrophotometry and gas chromatography, respectively. The highest extraction efficiency for fatty acids and pigments was achieved at 12.4 MPa, $35^{\circ}C$, $500{\mu}m$of seaweed size.

• Applied Chemistry for Engineering
• /
• v.9 no.1
• /
• pp.76-81
• /
• 1998

Physical adsorption on a silica gel(pore size of 80 nm, particle size of $10{\mu}m$)has been studied for binary mixture of acetone diluted in $CO_2$ by use of a FTIR transmission technique and we have compared the result of FTIR transmission technique with that of a chromatographic technique. Measurements were made at 313.2 K and under pressures up to 15MPa. As the pressure increases from 0.1MPa, the IA(Integral Absorbance) of the hydrogen-bonded OH groups interacting with acetone and adsorbed amount by use of a chromatographic technique increases at first, and reaches a maximum at a pressure below the critical pressure of $CO_2$, and then the intensities decrease gradually with increasing pressure. It is found that the pressure dependency of the chromatographic isotherm is a little larger than that of spectroscopic isotherm in the supercritical fluid region. This difference might be attributable to the weaker van der Waals force and relatively stronger hydrogen-bonding force influencing the adsorption of acetone on the sllica gel. The unique spectroscopic characteristics of amine group which vibrational frequencies of hydroxyl groups on the silica gel surface shift downward to about $1300cm^{-1}$ were measured from experimental result of triethylamine diluted in $CO_2$ or $N_2$.