• Bulletin of the Korean Chemical Society
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• v.4 no.4
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• pp.183-188
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• 1983

Two major and two minor polyacetylenes were isolated from fresh white Korean ginseng roots. The petroleum ether-ethyl ether fractions containing the polyacetylene compounds were collected through solvent fractionation, partition and silica gel column chromatography. Further separation of polyacetylenic fractions was proceeded by bonded normal phase HPLC utilizing a moderately nonpolar microparticulate column. The low pressure liquid chromatography was used for the semi-preparative separation. The chemical structures of the two major polyacetylenes separated were determined by UV, IR, $^1H$ NMR, $^{13}C$ NMR, mass spectra and elemental analysis. One of them is identified to be heptadeca-1-en-4, 6-diyne-3, 9, 10-triol, a new structure, and the other is heptadeca-1, 9-dien-4, 6-diyn-3-ol, known as panaxynol.

• Korean Journal of Pharmacognosy
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• v.24 no.4
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• pp.309-312
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• 1993

A new method for separation and quantitative determination of isoflavone glucosides in rhizomes of Belamcanda chinensis (Iridaceae) by high performance liquid chromatography was elaborated. A reverse-phase system with a Spheri-5 RP-18 column using MeOH:HOAc:$H_2O$(24 : 5 : 71) as a mobile phase was developed. The isoflavonoids were detected at 268 nm and the analysis was successfully carried out within 15 min.

• Analytical Science and Technology
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• v.37 no.5
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• pp.306-314
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• 2024

This study describes the liquid chromatographic enantiomer separation of three typical chiral amines (α-methylbenzylamine, 2-amino-4-methyl-1-pentanol, and 1-methylheptylamine) as 2-hydroxynaphthaldimine derivatives using six amylose trisphenylcarbamates derived chiral stationary phases (CSPs). It was observed that the structural nature of three chiral amines and the structures of amylose chiral selectors can affect their chiral recognition ability. Among the three analytes as 2-hydroxynaphthaldimine derivatives, in general, the greatest enantioselectivities of aromatic amine analyte (α-methylbenzylamine) were achieved on amylose trisphenylcarbamate derived CSPs and were followed by amino alcohol analyte (2-amino-4-methyl-1-pentanol), and aliphatic amine analyte (1-methylheptylamine). Also, the enantiodiscrimination abilities obtained on the two CSPs, Chiralpak ID and Chiralpak IF, were selectively higher than the other four amylose trisphenylcarbamate derived CSPs for the studied analytes. The underlying chiral recognition mechanism between 2-amino-4-methyl-1-pentanol as 2-hydroxynaphthaldimine derivatives and amylose tris(3,5-dimethylphenylcarbamate) chiral selector of Chiralpak AD-H and Lux Amylose-1 was elucidated by molecular docking study, and it was observed that the intermolecular hydrogen bonding interactions by hydroxyl moiety on the amino alcohol analyte as 2-hydroxynaphthaldimine derivatives were the main interactive forces driving the chiral separation. The obtained binding energies between 2-amino-4-methyl-1-pentanol analyte as 2-hydroxynaphthaldimine derivative and amylose tris(3,5-dimethylphenylcarbamate) chiral selector were in agreement with the experimentally determined enantioseparation and elution order by chiral HPLC.

• Analytical Science and Technology
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• v.25 no.6
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• pp.460-466
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• 2012

An environmentally friendly, so-called green, high performance liquid chromatography method was developed and validated for the determination of trans, trans-muconic acid (t,t-MA) in human urine as a biomarker of benzene exposure. After urinary t,t-MA was extracted and enriched using solid-phase extraction, a MF-Ph1 SG80 ($150mm{\times}2.0mm$ I.D., 5 ${\mu}m$) column with a mobile phase of 10 mM $KH_2PO_4$ containing 0.1% $H_3PO_4$ was used for isocratic separation of t,t-MA with UV detection at 259 nm. The calibration curve was constructed in the range of 0.1-5.0 mg/L with good linearity ($r^2$=0.9992). The intra-day and inter-day precision (as RSD) were 0.9-8.5% and 3.1-4.5%, respectively. The average recovery ranged from 97.5% to 101.7%. The green sample preparation and separation with no organic solvents were successfully achieved. The validated method would be suitable for the routine biological monitoring of benzene exposure in the occupational settings.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.6 no.1
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• pp.28-37
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• 1996

Benzidine, an aromatic amine used primarily in the manufacture of azo dyes, is recognized as a urinary bladder carcinogen in humans. In rats, mice, and hamsters, chronic exposure to benzidine resulted in tumors of the liver. The present study was undertaken to suggest analyzing the metabolites of benzidine with the optimal condition, identify the metabolites of benzidine, and observe time variance of the metabolites in the isolated perfusated rat liver. N-acetylbenzidine was synthesized by acetylation of benzidine with acetic anhydride and separated by thin layer chromatography(TLC) and high performance liquid chromatography(HPLC). To analysis benzidine and the metabolites of benzidine, HPLC operating condition has been optimized by means of preliminary experiment. The mobile phase consisted of acetonitrile(37%) in phosphate buffer, flow rate maintained at 1.0 ml/min. Optimal detective conditions were electrochemicaldetector(ECD) at 0.75 V for benzidine and N-acetylbenzidine and ultravioletdetector(UVD) at 287 nm for N,N'-diacetylbenzidine. The separation system was composed of a guard column and a separation column(Polymer C18, $4.6{\times}250cm$) at a temparature of $40^{\circ}C$. The perfusion system was equilibrated for 30 minutes before addition of benzidine to the perfusate. Samples of the perfusate were collected at time intervals(0, 10, 20, 30, 60, 90, 120 min) during the 2 hour perfusion. Before analyzing samples by HPLC/ECD/UVD, samples had been treated with sep-pak. Samples of perfusate analyzed by HPLC/ECD/UVD and the metabolites of benzidine in the isolated perfused rat liver were N-acetylbenzidine and N,N'-diacetylbenzidine. Benzidine metabolized over 60% during the initial 30 minutes of perfusion, extensively by 1 hour, and was undetectable in the perfusate. N-acetylbenzidine increased by 30 minutes of perfusion, declined. N,N'-diacetylbenzidine increased the 0-90 minutes period, remained constant during the 90-120 minutes period.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.35 no.1
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• pp.11-17
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• 2009

Betamethasone propionate, an anti-inflammatory glucocorticosteroid, was detected in cosmetics with no indication on the label of this compound as an ingredient. The product was formulated as a topical spray or shampoo and labeled to contain zinc pyrithione as the active ingredient. A thin-layer chromatographic analysis was carried out on silica gel plates to provide a first indication about the presence of a compound with steroid structure and reactivity; then high-performance liquid chromatography (HPLC) separation allowed the identification of the corticosteroid agent and its quantification. To identify the corticosteroid agent from these commercial samples we collected the fractions suspected to have ketol steroids by prep HPLC and identified the compound as betamethasone propionate by NMR and MS spectrometry. Then we synthesized the standard for the betamethasone 17-propionate and 21-propionate and quantitate the corticosteroids from the sample by HPLC with that standards. By this method we identified the corticosteroid compounds from some commercial cosmetics such as zinc pyrithione sprays. The finding of betamethasone propionate in the products was shown by comparison to an authenticated standard of betamethasone propionate by retention time on reverse-phase HPLC. Two of the tested products contained betamethasone propionate at the levels of 0.005 ${\sim}$ 0.02% and the others were free of betamethasone propionate.

• Analytical Science and Technology
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• v.20 no.4
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• pp.347-354
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• 2007

A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in bovine, porcine, chicken, flatfish and japanese eel muscle has been developed and validated. The separation condition for HPLC/UV was optimized with phenyl hexyl ($4.6{\times}150mm$, $5{\mu}m$) column with 10 mM monobasic sodium phosphate buffer (pH 2.5)/acetonitrile (50/50, v/v) as the mobile phase at a flow rate of 1.0 mL/min and detection wavelength was set at 254 nm. Residues were extracted from tissue by blending with methanol and lipid materials were removed with n-hexane. Then, the methanol extract was evaporated to dryness under a nitrogen stream, reconstituted in the mobile phase. Aliquot of the organic extract was decanted and filtered through $0.45{\mu}m$ syringe filter. The $20{\mu}L$ of the resulting solution was injected into the HPLC system. The calibration ranges were $0.5{\sim}5{\mu}g/g$ and calibration curves were linear with coefficients of correlation better than 0.95. The limits of quantification were $0.5{\mu}g/g$ for all muscles. The recoveries of bovine, porcine, chicken, flatfish and japaneseel muscles were 99.8%, 102.4%, 91.0%, 104.0% and 93.0%, respectively. The procedures were validated according to the CODEX guideline, determining specificity, linearity, accuracy, precision, quantitation limit and recovery.

• Journal of the Korean Society of Food Science and Nutrition
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• v.33 no.3
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• pp.549-552
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• 2004

A simple, efficient and accurate method was developed for the simultaneous determination of non-permitted oil soluble colorants (sudan I, II, III and IV) in foods. The identification has been carried out for sudan colorants by TLC as well as HPLC with photodiode array (PDA) detection. Separation of sudan colorants was achieved within 20 min by a gradient elution with water and acetonitrile as eluents. Sudan colorants showed good linear relationships in the range of 0.1 ～ 100 $\mu\textrm{g}$/mL. The correlation coefficients of the calibration curve for sudan colorants exceeded 0.999. The detection limits (signal-to-noise ratio 3 : 1) for sudan I, II, III and IV were 0.01, 0.01, 0.02 and 0.02 $\mu\textrm{g}$/mL, respectively. This method has been successfully applied to the analysis of red pepper powder, Kimchi and Kakdugi, and the average recoveries for real samples ranged from 83.02% to 104.3%.

• Journal of Environmental Health Sciences
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• v.22 no.1
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• pp.36-44
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• 1996

A comparison was made of two detection methods(UV absorbence detection and fluorescence detection with pre-column derivatization, with trifluoroacetic acid) coupled with HPLC for the simultaneous determination of aflatoxin $B_1, B_2, G_1$ and $G_2$. A good separation of the four aflatoxins was achieved on a reversed-phase $C_{18}$ column (30 cm x 3.9 mm) with methanol-acetonitrile-water(20+20+60) for absorbence detection or acetonitrile-water(25+75) for fluorescence detection at the flow rate of 1.0 ml/min. The calibration graphs were linear over the ranges 100 ppb-1 ppm for $B_1/G_1$ and 30~300 ppb for $B_2/G_1$ with absorbence detection, and 1~500 ppb for $B_1/G_1$ and 0.3~150 ppb for $B_2/G_2$ with fluorescence detection. The correlation coefficients were greater than 0.94 and 0.99 for absorbance detection and for fluorescence detection, respectively. The detection limit was 100 ng for $B_1/G_1$ and 30 ng for $B_2/G_2$ with absorbence detection, and 1 ng for $B_1/G_1$ and 0.3 ng for $B_2/G_2$ with fluorescence detection. Recovery rates of aflatoxin $B_1, B_2, G_1$ and $G_2$ added to yeast-extract sucrose broth medium were 66.6%, 59.4%, 67.5% and 59.2%, respectively, for absorbence detection and 82.9%, 71.5%, 80.0% and 69.3%, respectively, for fluorescence detection. The four aflatoxins in culture medium were quantitatively detected by the two methods. The aflatoxins in the rice sample were not detected the absorbence detection method, but were below 10 ppb using the fluorescence detection method. Analysis of aflatoxins by both the absorbence and fluorescence methods coupled with HPLC showed acceptable linearity and good recovery. The absorbence detection was less timeconsuming and safer for treatment. The fluorescence detection was more elective and sensitive though elevated $B_1$ and $G_1$ contents were determined from the TFA-induced conversion of $B_1$ to $B_{2a}$ and $G_1$ to $G_{2a}$.

• Natural Product Sciences
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• v.14 no.3
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• pp.147-151
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• 2008

A high performance liquid chromatographic (HPLC) method for the simultaneous determination of marker constituents, baicalin and glycyrrhizin was established for the quality control of traditional herbal medicinal preparation, Eul-Ja-Tang (EJT). Separation and quantification were successfully achieved with a Waters XTerra RP18 column ($5{\mu}m$, 4.6 mm I.D. ${\times}$ 150 mm) by gradient elution of a mixture of acetonitrile and water containing 0.03% phosphoric acid (pH 2.03) at a flow rate of 1.0 mL/min. The diode-array UV/VIS detector (DAD) was used for the detection and the wavelength for quantification was set at 250 nm. The presence of baicalin and glycyrrhizin in this decoction was ascertained by retention time, spiking with each authentic standard and UV spectrum. Both baicalin and glycyrrhizin showed good linearity ($r^2$ > 0.999) in a relatively wide concentration ranges. The R.S.D. for intra-day and inter-day precision was less than 5% and the limits of detection (LOD) were about 30 ng. The mean recovery of each compound was 99.5 - 101.2% with R.S.D. values less than 4.0%. This method was successfully applied to the determination of contents of baicalin and glycyrrhizin in three commercial products of EJT, which resulted in the difference in the contents of these compounds. These results suggest that the developed HPLC method is simple, effective and could be readily utilized as a quality control method for commercial EJT products.