• Korean Chemical Engineering Research
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• v.47 no.1
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• pp.54-58
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• 2009

Ketoprofen and ibuprofen are non-steroid anti-inflammatory drug(NSAID) that have analgesic and antipyretic properties. (S)-ketoprofen and (S)-ibuprofen have pharmacological activity, while (R)-ketoprofen and (R)-ibuprofen are either inactive or have side effect. The chiral separation of racemic ketoprofen and ibuprofen enantiomers was carried out by using a Kromasil HPLC column. Some chromatographic parameters (selectivity, resolution, number of theoretical plates and ${\Delta}H$) are calculated under different mobile phase compositions of hexane/t-BME/acetic acid and temperatures. The selectivity, resolution and number of theoretical plates were observed high at $25^{\circ}C$ and the composition of hexane/t-BME/acetic acid (80/20/0.1).

• KSBB Journal
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• v.20 no.3
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• pp.244-249
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• 2005

Chiral separation of racemic ibuprofen was achieved on a Kromasil KR100-5CHI-TBB column. Some chromatographic parameters (resolution, number of theoretical plates, HETP, capacity factor) are calculated under different separation conditions such as change of mobile phase compositions (hexane / t-BME : 85 / 15, 75 / 15, 65 / 35, 55 /45) as well as acetic acid concentrations for adjusting pH (0.1 to 1 $v/v\%$). Flow rate versus number of theoretical plates and HETP were compared to evaluate column efficiency. To determine the adsorption isotherms, PIM (Pulsed Input Method) was carried out. At concentrations of racemic ibuprofen between 0.1 and 0.3 mg/ml, S- and R-ibuprofen have the same retention time of 4.48 and 5.81 min. Ibuprofen isotherms show a linear form under concentrations of 0.3 mg/ml with eluent (hexane / t-BME = 55 / 45).

• Korean Chemical Engineering Research
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• v.46 no.4
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• pp.681-685
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• 2008

Chiral separation of racemic mandelic acid was achieved on a Kromasil KR100-5CHI-TBB column. Some chromatographic parameters (resolution, number of theoretical plates, capacity factor) are calculated under different separation conditions such as changes of mobile phase compositions (hexane/t-BME = 85/15 - 10/90) as well as formic acid concentrations for adjusting pH (0.1, 0.5, 1.0 v/v%). Flow rate versus number of theoretical plates was compared to evaluate column efficiency. To determine the adsorption isotherms, PIM (Pulse Input Method) was carried out. At the concentrations of racemic mandelic acid between 0.1 and 0.3 mg/ml, L- and D-mandelic acids have the same retention times of 8.8 and 9.4 min respectively. Mandelic acid isotherms show a linear form under the concentrations of 0.3 mg/ml with eluent (hexane/t-BME = 75/25). As the concentrations of mandelic acids increase, nonlinear Langmuir isotherms were observed as $C_{S,L}=3.358C_{M,L}/(1+0.0897C_{M,L})$ for L-mandelic acid and, $C_{S,D}=3.692C_{M,D}/(1+0.1457C_{M,D})$ for D-mandelic acid.

• KSBB Journal
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• v.18 no.4
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• pp.261-265
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• 2003

Ibuprofen was analyzed by chiral high performance liquid chromatography. Retention behaviours of the standard mixtures of ibuprofen were investigated to obtain their acceptable resolution. A chromatographic column (3.9 ${\times}$ 300 mm) was packed by Kromasil CHI-TBB packings (10 $\mu\textrm{m}$) and n-hexane was used as a mobile phase with 0.1％ acetic acid and tert-butyl methyl ether. Isocratic elution of ibuprofen at 1.0 $m\ell$/min was performed by changing the mobile phase compositions. The experimental variables affecting the resolution were the compositions of mobile phase and chemical buffer (n-hexane and tert-butyl methyl ether). The resolution between the enantiomers were correlated into the several types of empirical equations including linear form, and their agreements between experimental data and calculated values were examined by the regression coefficient.

• Bulletin of the Korean Chemical Society
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• v.25 no.12
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• pp.1807-1811
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• 2004

Supercritical fluid chromatography (SFC) was considered for separating racemic ibuprofen. The chromatographic column (3.9 ${\times}$ 150 mm) was packed with Kromasil$^{\circledR}$ CHI-TBB, and the mobile phase was supercritical carbon dioxide with modifier of IPA. The experimental variables were the content of IPA, and temperature and pressure of supercritical mobile phase. To determine the separation condition, the empirical equation of retention factor and resolution was proposed. In the case of retention factor, the empirical equation was in the form, $k\;=\;a{\rho}\;+b/F\;+\;c\;({\rho}/F)\;+\;d$. The empirical equation for resolution was proposed as a linear form, $R\;=\;a{\rho}\;+\;bF\;+\;c$.

• Korean Journal of Pharmacognosy
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• v.45 no.1
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• pp.84-87
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• 2014

A high performance liquid chromatography (HPLC) method for the quantitation of ellagic acid in Nymphaea tetragona was developed for the quality control of functional cosmetic ingredient, the extract of N. tetragona. Separation and quantitation were successfully achieved with a Kromasil C18 column ($5{\mu}m$, $250mm{\times}4.6mm$, i.d.) by isocratic elution of a mixture of acetonitrile containing 0.1% trifluoroacetic acid and water containing 0.03% phosphoric acid at a flow rate of 1.0 ml/min. The UV detector was used for the detection and the wavelength for quantitation was set at 254 nm. The presence of ellagic acid in the extract was determined by comparison of retention time and spiking with authentic standard. Analytical results showed good linearity ($R^2=0.99996$) in relatively wide concentration ranges. The R.S.D. for precision test was less than 3.0%. Recovery of the compound was 98.55~101.72% with R.S.D values less than 4.0%. In conclusion, this method has been successfully applied to the determination of ellagic acid in N. tetragona.

• YAKHAK HOEJI
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• v.57 no.4
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• pp.272-281
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• 2013

In this study, we developed and validated the HPLC method using the isolated components from Erycibae caulis. Their structures were elucidated by spectroscopic methods including UV, $^1H$-NMR, $^{13}C$-NMR, FAB-Mass and ESI-Mass as Compound 1 (crypto-chlorogenic acid), Compound 2 (scopolin), Compound 3 (neochlorogenic acid) and Compound 4 (3,4-di-O-caffeoylquinic acid). Major three compounds and scopoletin were decided as representative components of Erycibae caulis. We established HPLC analytical method by using the representative components and 20 commercial samples which were collected considering to various cultivated area. The HPLC fingerprinting was successfully achieved with an AKZO NOBEL Kromasil 100-5C18 column. The mobile phase consisted of 0.5% acetic acid in water (A) and methanol (B) using gradient method of 85(A) to 50(A) for 35min. The fingerprints of chromatograms were recorded at an optimized wavelength of 330 nm. This developed analytical method was validated with specificity, selectivity, accuracy and precision. And it is suggested that scopolin, scopoletin, neochlorogenic acid, 3,4-di-O-caffeoylquinic acid were more than 0.162%, 0.133%, 0.057%, 0.044%, respectively. In addition, principal component analysis (PCA) was performed on the analytical data of 20 different Erycibae caulis samples in order to classify samples collected from different regions. We hope that this assay can be readily utilized as quality control method for Erycibae caulis.

• Journal of the Korean Society of Food Science and Nutrition
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• v.45 no.11
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• pp.1604-1609
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• 2016

An HPLC analysis method was developed for standard determination of marmesin as a functional health material in Broussonetia kazinoki extract. HPLC was performed on a $C_{18}$ Kromasil column ($4.6{\times}250mm$, $5{\mu}m$) with a gradient elution of 0.1% (v/v) trifluoroacetic acid and acetonitrile at a flow rate of 1.0 mL/min at $30^{\circ}C$. The analyte was detected at 330 nm. The HPLC method was validated in accordance with International Conference on Harmonization guidelines for analytical procedures with respect to specificity, precision, accuracy, and linearity. The limit of detection and quantitation were 6.2 and $18.6{\mu}g/mL$, respectively. Calibration curves showed good linearity ($r^2$>0.9999), and the precision of analysis was satisfactory (less than 0.3%). Recoveries of quantified compound ranged from 100.35 to 101.18%. This result indicates that the established HPLC method is very useful for the determination of marker compounds in B. kazinoki extracts.

• Journal of the Korean Society of Food Science and Nutrition
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• v.45 no.1
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• pp.61-67
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• 2016

An HPLC analysis method was developed for standard determinations of chlorogenic acid, 3,4-di-O-caffeoylquinic acid, 3,5-di-O-caffeoylquinic acid, and 4,5-di-O-caffeoylquinic acid as functional health materials in Ligularia fischeri extract. HPLC was performed on a $C_{18}$ Kromasil column ($4.6{\times}250mm$, $5{\mu}m$ column) with a gradient elution of 0.1% (v/v) trifluoroacetic acid and acetonitrile at a flow rate of 1.0 mL/min at $30^{\circ}C$. The analytes were detected at 330 nm. The HPLC method was validated in accordance with the International Conference on Harmonization guideline of analytical procedures with respect to specificity, precision, accuracy, and linearity. The limits of detection and quantitation for the four compounds were 3.0~14.6 and $9.2{\sim}44.4{\mu}g/mL$, respectively. Calibration curves showed good linearity ($r^2$ > 0.999), and the precision of analysis was satisfied (less than 0.9%). Recoveries of quantified compounds ranged from 98.96 to 101.81%. This result indicates that the established HPLC method is very useful for the determination of marker compounds in Ligularia fischeri leaf extracts.