• Analytical Science and Technology
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• v.14 no.3
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• pp.244-252
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• 2001

A comprehensive analytical method of endocrine distruptors[i.e., nonylphenol(NP), octylphenol(OP), bis(2-ethylhexyl)phthalate(BEHP)] is fish samples was developed using two internal standards. This method employed closed culture tube extraction with dichloromethane and solvent exchange to iso-hexane and SPE(2g) aminopropyl column, followed by determination on gas chromatograph linked to mass spectrometer(GC/MS) operated in the single ion monitoring(SIM) mode. The recoveries of nonylphenol and octyphenol in the range of $0.2{\sim}20{\mu}g/g$ using 1-phenyl decanol as one internal standard were over 75%, and recovery of bis(2-ethylhexyl)phthalate in the range of $0.4{\sim}40{\mu}g/g$ using bis(2-ethylbutyl)phthalate(BEBP) as the other internal standards was showed over 102%. The present method was applied to fish samples from Korea and UK. The range of concentrations for nonylphnol(NP) and bis(2-ethylhexyl)phthalate in Korean fish were $0.02{\sim}0.06{\mu}g/g$ in 2 samples and $0.18{\sim}2.03{\mu}g/g$ in 9 samples respectively, but bis(2-ethylhexyl)phthalate(BEHP) in UK samples was found $2.99{\mu}g/g$ in just 1 sample. But octylphenol(OP) was not dected in any samples by this method. This two internal standard method provides a more precise analytical tool to investigate endocrine disruptors in a biological matrices of limited quantity.

• Journal of Pharmaceutical Investigation
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• v.40 no.2
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• pp.101-107
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• 2010

A rapid and sensitive reversed-phase high performance liquid chromatography (HPLC) method was developed for the determination of N-(-4-Chlorophenyl)-6-hydroxy-7-methoxy-2-chromanecarboxamide (KAL-1120), a novel anti-inflammation agent, in the rat plasma. The method was applied to analyze the compound in the biological fluids such as bile, urine and tissue homogenates. After liquid-liquid extraction, the compound was analyzed on an HPLC system with ultraviolet detection at 275 nm. HPLC was carried out using reversed-phase isocratic elution with a $C_{18}$ column, a mobile phase of a mixture of acetonitril (40 v/v%) at a flow rate of 1.0 mL/min. The chromatograms showed good resolution and sensitivity and no interference of plasma. The calibration curve for the drug in plasma was linear over the concentration range of 0.05-50 ${\mu}g$/mL. The intra- and inter-day assay accuracies of this method ranged from 0.06% to 9.33% of normal values and the precision did not exceed 6.28% of relative standard deviation. The plasma concentration of KAL-1120 decreased to below the quantifiable limit at 1.5 hr after the i.v. bolus administration of 2-10 mg/kg to rats ($t_{1/2,({\alpha})}$ and $t_{1/2,({\beta})$ of 2.15 and 26.7 min at a dose of 2 mg/kg, 3.91 and 33.0 min at a dose of 10 mg/kg, respectively). The steady-state volume of distribution ($V_{dss}$) and the total body clearance ($CL_t$) were not significantly altered in rats given doses from 2 to 10 mg/kg. Of the various tissues tested, KAL-1120 was mainly distributed in the lung and heart after i.v. bolus administration. KAL-1120 was detected in the bile by 30 min after its i.v. bolus administration. However, the concentration in the urine after i.v. bolus administration became too low to measure, suggesting that KAL-1120 is mostly excreted in the bile. In conclusion, this analytical method was suitable for the preclinical pharmacokinetic studies of KAL-1120 in rats.

• Journal of Food Hygiene and Safety
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• v.32 no.5
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• pp.418-423
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• 2017

An analytical method for the determination of dexamethasone (DM) in bovine milk samples was developed and validated using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Milk samples were extracted by the liquid-liquid extraction based on acetonitrile. The chromatographic separation was achieved on a reverse phase $C_{18}$ column with gradient elution using a mobile phase of 0.1% formic acid in 95% acetonitrile. The procedure was validated according to the Ministry of Food and Drug Safety guideline determining accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ). Mean recoveries of DM from spiked milk samples (25, 125, and 1,250 ng/mL) were 98.9-109.6%, and the relative standard deviation was between 1.7 and 4.4%. Linearity in concentration range of 12.5-1,250 ng/mL was obtained with the correlation coefficient ($r^2$) of 0.9997. LOD and LOQ for the investigated DM were 0.15 and 0.5 ng/mL depending on milk samples, respectively. This method was reliable, sensitive, economical and suitable for routine monitoring of DM residues in bovine milk.

• Korean Journal of Food Science and Technology
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• v.43 no.3
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• pp.277-281
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• 2011

A rapid and very sensitive high-performance liquid chromatography/atmospheric-pressure chemical-ionization mass spectrometry method to detect ethylenethiourea (ETU) fungicide residues in fruits was developed. Methylene chloride was used as the surface extraction solvent for the target component. Recovery rates improved when cysteine hydrochloride and sodium carbonate were added to product prior to fortification. The limits of detection and quantification were approximately 0.006 and 0.02 mg/kg, respectively, from mandarin oranges. Recoveries from mandarin oranges, oranges, bananas, and pears, spiked in the range of 0.05-0.5 mg/kg, averaged 80-100%. The proposed method was used to monitor the presence of ETU in commercial fruits purchased from different markets in Seoul, Korea. ETU was found in four orange peels and in three mandarin orange peel samples. The highest ETU residue levels were $73.6{\mu}g/kg$ and $29.8{\mu}g/kg$.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.15 no.8
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• pp.5393-5399
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• 2014

To examine the effects of a mycosporine-like amino acids (MAAs) mixture from microalgae, Chlamydomonas sp, on the anti-wrinkle activities, the expression levels of genes that are associated with skin aging, including type I procollagen, elastin and involucrin, were analyzed. Asterina 330+palythine (A+P) and shinorine+palythine (S+P) mixtures were purified from Chlamydomonas sp using the following steps: 80% methanolic extraction, column purification, and HPLC analysis. As a result of the MTT assay, A+P and S+P did not induce cellular cytotoxicity with up to 0.1 mg/mL of both MAAs. In addition, the treatment of UV-exposed fibroblasts with A+P (0.05 mg/mL) and S+P (0.01 mg/mL) increased the levels of the PCOLCE mRNAs by 2.7 and 3.6 fold compared to the control group, respectively, The levels of elastin gene expression were elevated 5.59 and 3.1 fold in the A+P and S+P treated (0.01 mg/mL) cells, respectively. In particular, at a concentration of 0.01 mg /mL, the A+P and S+P expression levels of Involucrin mRNAs were increased 3.5 and 2.5 fold in the UV-exposed cells compared to the control, respectively. In conclusion, the MAAs derived from Chlamydomonas sp can be utilized as functional cosmetic materials with anti-wrinkle effects on the skin.

• Journal of Food Hygiene and Safety
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• v.25 no.2
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• pp.118-121
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• 2010

A HPLC-MS/MS method was developed for simultaneous determination of six sweeteners (acesulfame-K, cyclamate, saccharin, sucralose, stevioside, aspartame) in children's favorite foods. The procedure involves an extraction of the six sweeteners with 50% methanol solution, sample clean-up using the Carrez clearing reagent and filtering with cartridge filter. The HPLC separation was performed on a Hypersil Gold (150 mm ${\times}$ 2.1 mm 5 um) column using the water/acetonitrile mobile phase (95:5). Mass spectrometric analysis was carried out using the TSQ Quantum Ultra operated in negative and positive ESI/SRM. With this method, good linear relationship, sensitivity and reproducibility were obtained. The spike recoveries of six sweeteners for 2 kinds of foods spiked into 0.4 mg/ kg ranged from 87.4 to 114.7%. The detection limits were above 0.02 mg/kg. The method has been applied to determination of six sweeteners in children's favorite foods.

• Journal of Life Science
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• v.24 no.8
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• pp.860-864
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• 2014

PAP-1, a novel antimicrobial peptide isolated from pyloric caeca extract of the starfish Asterina pectinifera was purified and characterized. First, the acidified pyloric caeca extract was put through Sep-Pak C18 solid phase extraction cartridge using a stepwise gradient. Among the eluents, RM 60 (retained materials at 60% methanol) showed good antimicrobial activity against Bacillus subtilis and Escherichia coli D31 and was purified in C18 reversed-phase and ion-exchange high-performance liquid chromatography columns. The purification steps yielded two novel peptides showing strong antimicrobial activities. These peptides were named pyloric caeca A. pectinifera peptide 1 and 2 (PAP-1 and PAP-2). For the characterization of the purified peptides, the molecular weights and amino acid sequences were determined by MALDI-TOF MS and Edman degradation. The molecular weights of PAP-1 and PAP-2 were about 2951.54 Da and 2980.15 Da respectively. The amino acid sequences of PAP-1 and PAP-2 were partially determined: AIQNAGES and AIQNAAES, respectively. PAP-2 is an isoform of PAP-1, differing merely by a single residue at position 6 (glycine or alanine). The comparison of the N-terminal amino acid sequences and molecular weights of the peptides with those of other known antimicrobial peptides revealed that PAP-1 and PAP-2 have no homology with any known peptides. These findings suggest that PAP-1 and PAP-2 play a significant role in the innate defense system of starfish pyloric caeca.

• The Korean Journal of Pesticide Science
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• v.18 no.3
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• pp.141-147
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• 2014

Fenpyroximate is acaricide of pyrazole group. This acaricide have already been permitted for herb cultivation. This experiment was conducted to establish a determination method for fenpyroximate residue in herbal medicines using HPLC-PDA and HPLC-MS/MS. Fenpyroximate residue was extracted with acetone from samples of herbal which Liquorice Root (Glycyrrhiza uralensis) and Safflower Seed (Carthamus tinctorius Linne). The extract was diluted with saturated saline water and dichloromethane liquid-liquid partition (extraction) was followed to recover fenpyroximate from the aqueous phase. Amino propyl ($NH_2$) and florisil column chromatography was additionally employed for final clean up of the extract. The fenpyroximate was quantitated by HPLC-PDA and HPLC-MS/MS. The herbals were fortified with fenpyroximate at 2 or 3 levels per crop. Mean recovery ratio were ranged from 72.0 to 106.4%. The coefficients of variation were ranged from 0.2 to 4.4. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fenpyroximate in herbal medicines.

• Microbiology and Biotechnology Letters
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• v.42 no.3
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• pp.219-224
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• 2014

In order to develop a new anti-diabetic ${\alpha}$-glucosidase inhibitor, we compared the ${\alpha}$-glucosidase inhibitory activity of the cell-free extracts of 48 strains of yeasts isolated from Korean fermented foods, and found that Pichia burtonii Y257-7 exhibited the highest ${\alpha}$-glucosidase inhibitory activity of 55.6%. The ${\alpha}$-glucosidase inhibitor was maximally produced when Pichia burtonii Y257-7 was cultured in LB broth (initial pH of 6.0) at $28^{\circ}C$ for 24 h. The ${\alpha}$-glucosidase inhibitor, partially purified by Sephadex G-50 gel permeation chromatography and systematic solvents extraction, revealed potent hypoglycemic effects in normal rats and streptozotocin-induced diabetic rats after the oral administration of starch.

• Bulletin of the Korean Chemical Society
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• v.30 no.5
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• pp.1121-1126
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• 2009

This paper describes a pattern recognition method of Magnoliae flos based on a gas chromatographic/mass spectrometric (GC/MS) analysis of the essential oil components. The botanical drug is mainly comprised of the four magnolia species (M. denudata, M. biondii, M. kobus, and M. liliflora) in Korea, although some other species are also being dealt with the drug. The GC/MS separation of the volatile components, which was extracted by the simultaneous distillation and extraction (SDE), was performed on a carbowax column (supelcowax 10; 30 m{\time}0.25 mm{\time}0.25{\mu}m$) using temperature programming. Variance in the retention times for all peaks of interests was within RSD 2% for repeated analyses (n = 9). Of the 74 essential oil components identified from the magnolia species, approximately 10 major components, which is $\alpha$-pinene, $\beta$-pinene, sabinene, myrcene, d-limonene, eucarlyptol (1,8-cineol), $\gamma$-terpinene, p-cymene, linalool, $\alpha$-terpineol, were commonly present in the four species. For statistical analysis, the original dataset was reduced to the 13 variables by Fisher criterion and factor analysis (FA). The essential oil patterns were processed by means of the multivariate statistical analysis including hierarchical cluster analysis (HCA), principal component analysis (PCA) and discriminant analysis (DA). All samples were divided into four groups with three principal components by PCA and according to the plant origins by HCA. Thirty-three samples (23 training sets and 10 test samples to be assessed) were correctly classified into the four groups predicted by PCA. This method would provide a practical strategy for assessing the authenticity or quality of the well-known herbal drug, Magnoliae flos.