• Bulletin of the Korean Chemical Society
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• v.34 no.6
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• pp.1684-1688
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• 2013

A rapid and sensitive method for determining usnic acid of Lethariella cladonioides in rat was established using high performance liquid chromatography (HPLC) quadrupole time-of-flight (QTOF) tandem mass (MS/MS). Rat plasma was pretreated by mixture of acetonitrile and chloroform to precipitate plasma proteins. Chromatographic separation was achieved on a column ($50{\times}2.1$ mm, $5{\mu}m$) with a mobile phase consisting of water (containing $5{\times}10^{-3}$ M ammonium formate, pH was adjusted to 3.0 with formic acid) and acetonitrile (20:80, v/v) at a flow rate of 0.3 mL/min. A tandem mass spectrometric detection with an electrospray ionization (ESI) interface was conducted via collision induced dissociation (CID) under negative ionization mode. The MS/MS transitions monitored were m/z 343.0448 ${\rightarrow}$ m/z 313.2017 for usnic acid and m/z 153.1024 ${\rightarrow}$ m/z 136.2136 for protocatechuic acid (internal standard). The linear range was calculated to be 2.0-160.0 ng/mL with a detection limit of 3.0 pg/mL. The inter- and intra-day accuracy and precision were within ${\pm}7.0%$. Pharmacokinetic study showed that the apartment of usnic acid in vivo confirmed to be a two compartment open model. The method was fully valid and will probably be an alternative for pharmacokinetic study of usnic acid.

• KSBB Journal
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• v.15 no.4
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• pp.352-358
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• 2000

Preparation for the simplified separation of chitosandoligosaccharides from enzymatic hydrolysate was investigated. Two different types of chitosan beads as substrate were prepared as organic-based bead by W/O emulsion method and water-based bead by alkaline treatement. The average size of organic-based bead was $200{\mu}m$, and that of water based beads were $4000{\mu}m$, $100{\mu}m$, $30{\mu}m$, in diameter respectively. Enzyme stability was maintained over 80% at PH 6 after 24 hours. The optimal condition for the production of chitosanoligosaccharides was at pH 6.0, $50^{\circ}C$ and 40U (200U/g-chitosan) According to final oligosaccharide concentration water-based bed showed the similar result with that of organic-based bead even through it had smaller surface area attacked by chitosanse than that of organic-based bead. It is probable that the structure of water-based chitosan bead was looser than that of organic-based bead so enzyme penetrated easily into the bead structure. For the oligosaccharide production versus surface area the different size of water-based beads was investigated, Maxiaml production yield was observed in the $30{\mu}m$ beads. Consequently the water-based chitosan bead was better than the organic-based bead in this reaction system.

• Asian Journal of Atmospheric Environment
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• v.5 no.3
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• pp.146-151
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• 2011

1-Nitropyrene (1-NP), 2-NP and 2-nitrofluoranthene (2-NFR) are useful markers for studying the atmospheric behaviors of polycyclic aromatic hydrocarbons (PAHs) and nitropolycyclic aromatic hydrocarbons (NPAHs). However, present methods for measuring trace levels of these compounds are lesssensitive and laborious. Here we describe several improvements to a previously reported high-performance liquid chromatography-chemiluminescence detection system that allows it to determine trace levels of 1-, 2-NPs and 2-NFR. The proposed system was equipped with a reducer column packed with Pt/Rh instead of zinc whose life-time was limited. The combination of Cosmosil MS-II (monomeric ODS) and AR-II (polymeric ODS) columns was used instead of polymeric ODS columns as the separator column to improve the separation. An ethanol mixture with acetate buffer (pH 5.5) was used in place of an acetonitrile mixture with the same buffer to activate the reducer column. The same ethanol mixture was used as the mobile phase for the clean-up column. The switching time of the column switching valve was optimized to concentrate the amino-derivatives of above NPAHs quantitatively on the concentrator column. The concentrations of bis(2,4,6-trichlorophenly) oxalate and hydrogen peroxide in the chemiluminescence reagent solution were optimized to 0.4 mM and 30 mM, respectively, to increase the sensitivity. Under the above conditions, the detection limits (S/N=3) of 1-, 2-NPs and 2-NFR were 1 fmol (0.25 pg), 10 fmol (2.5 pg) and 4 fmol (1 pg), respectively. The proposed system was effectively used to determine trace levels of 1-, 2-NPs and 2-NFR in airborne particulates collected at Noto Peninsula. The atmospheric concentrations of 1-, 2-NPs and 2-NFR were not more than sub pg $m^{-3}$ levels. They were higher in winter (January) than in summer (July). In both seasons, the concentrations were in decreasing order, [2-NFR]>[1-NP]>[2-NP].

• Journal of Food Hygiene and Safety
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• v.22 no.4
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• pp.370-374
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• 2007

An analytical method for the simultaneous determination of four tetracycline (oxytetracycline, tetracycline, chlortetracycline, doxycycline) in egg samples was developed and validated using liquid chromatography with ultraviolet detection. Egg samples were extracted by the liquid-liquid extraction based on acetonitrile. The chromatographic separation was achieved on a reverse phase C8 column with gradient elution using a mobile phase of 20 mM oxalic acid (pH 1.5)/acetonitrile. The procedure was validated according to the Food Drugs Administration guideline determining accuracy, precision, and limit of detection. Mean recovery of tetracyclines from spiked egg samples (50, 100, 200, 400, and $800{\mu}g/kg$) were 78.8-109.3%. Linearity in concentration range of $50-800{\mu}g/kg$ was obtained with the correlation coefficient $(r^2)$ of 0.994-0.999. The intra- and inter-day precision (relative standard deviation; RSD) was between 0.3-12.8 and 0.2-11.7%, respectively. Limit of detection (LOD) and limit of quantification (LOQ) for the investigated tetracyclines were 30 and $50{\mu}g/kg$ depending on egg samples, respectively. This method was reliable, sensitive, economical and suitable for routine monitoring of tetracycline residues in dairy egg.

• Analytical Science and Technology
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• v.5 no.4
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• pp.389-399
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• 1992

Liquid Chromatographic behavior of Pd(II) in Isonitrosoethylacetoacetate lmine, $Pd(IEAA-NR)_2$ (R=H, $CH_3$, $C_2H_5$, $n-C_3H_7$, $C_6H_5-CH_2$, $n-C_4H_9$) chelates were investigated by reversed-phase HPLC on Micropak MCH-5 column using methanol/water as mobile phase. The optimum conditions for the separation of $Pd(IEAA-NR)_2$ chelates were examined with respect to the effect of the flow rate, sample solvent, mobile phase strength and column temperature. It wass found that metal chelates were properly eluted in an acceptable range of capacity factor value($0{\leq}log\;k^{\prime}{\leq}1$). The dependence of the logarithm of capacity factor(k') on the volume fraction of water in the binary mobile phase was examined. Also, the dependence of k' on the liquid-liquid extration distribution ratio($D_c$) in methanol-water/n-alkane extration system was investigated. Both kinds of dependence are linear, which susggests that the retention of the electroneutral metal chelate is largely due to the solvophobic effect. Standard adsorption enthalpy changes (${\Delta}H^{\circ}$) and standard adsorption entropy changes (${\Delta}S^{\circ}$) of Pd(II) Isonitrosoethylacetoacetate imine chelates on Micropak MCH-5 column were calculated by measuring capacity factor with changing temperature of the column.

• Analytical Science and Technology
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• v.24 no.2
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• pp.127-134
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• 2011

Quantitative HPLC analysis for the determination of in herbal liquid preparations was improved from the general test method besides the Korean Pharmacopeia. Good chromatographic separation of samples containing parabens, interferences, and other pharmaceutical excipients was effectively achieved by using acetonitrile water (containing 1% glacial acetic acid) mixture (30:70 v/v) as mobile phase. To monitor preservatives (benzoic acid, parabens, sorbic acid, dehydroacetic acid, and their salts) in herbal liquid preparations, a group of 47 samples was divided into two different group: preservative labeled group and unlabeled group. From the results, the contents of preservatives in 31 samples of preservative labeled group fell under KFDA regulations, and the contents of dehydroacetic acid in 6 samples of preservative labeled group were not followed by KFDA regulations. Preservatives were detected in 3 samples out of 10 samples in preservative unlabeled group.

• Korean Chemical Engineering Research
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• v.44 no.5
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• pp.453-459
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• 2006

D-tryptophan and N-CBZ-D-phenylalanine were separated using ionic liquid as additives for the mobile phase in high performance liquid chromatography (HPLC). The ionic liquid of 1-butyl-3- methylimidazolium tetrafluoroborate (${[BMIm]}^+{[BF_4]}^-$) was used. Mobile phases were 65％, 70％, and 80％ methanol in water with addition of different concentrations (0.5, 1.0, 1.5, 2.0, 4.0, 6.0, 8.0, 10.0, 12.0, and 15.0 mmol/L) of the ionic liquid. The experiments were performed on stainless steel column, $3.9{\times}300mm$ i.d., packed with $15{\mu}m$ octadecyl-bonded silica gel at laboratory.The retention factor of D-tryptophan was not negligibly changed while that of N-CBZ-D-phenylalanine was decreased. The resolution between the two components were affected by the contents of methanol and ionic liquid in the mobile phase. With the small content of methanol and the high concentration of ionic liquid, the resolution was improved.

• Journal of Environmental Health Sciences
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• v.42 no.1
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• pp.53-60
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• 2016

Objectives: Preservatives are commonly used in pharmaceuticals, cosmetics and other products to extend the expiration date and prevent the growth of microorganisms. Preservatives are generally effective in controlling mold and inhibiting yeast growth, and against a wide range of bacterial attacks as well. They also adversely affect the quality of sperm and cause precocious puberty in children. This study was performed to analyze seven preservatives used in pharmaceuticals and personal care products. Methods: Five kinds of pharmaceuticals and personal care products (PPCPs) were examined for analysis with a high performance liquid chromatography-diode array detector. Each sample was homogenized and the targeted compounds were extracted with methanol. The suspended particulate was removed by syringe filter. Next, the sample was injected into an HPLC system. The separation of the seven preservatives was achieved with a C18 column and gradient mode. The accuracies were between 73% and 120% and precision was lower than 11.58% (RSD). Results: All of the calibration curves showed good linearity with a coefficient of determination ($r^2$) over 0.999. Among the PPCP samples, the detection rate of preservatives was 32.5% for pharmaceuticals, 44.8% for toothpaste, 76.9% for mouthwash, 40.0% for body lotion and 56.0% for wet tissues. The average concentrations of the preservatives in PPCPs were BA 1141.0 mg/kg, MP 709.8 mg/kg, EP 624.9 mg/kg, PP 216.9 mg/kg, BP 167.8 mg/kg, and TCS 538.2 mg/kg. The most frequently detected preservatives in pharmaceuticals and personal care products were BA, MP and PP. The concentrations of preservatives exceeded Korean regulatory standards in 11 samples of medicines, three of mouthwash and two of body lotion. Conclusion: We found that most of the PPCP samples contained various preservatives. It is necessary to identify which preservatives were used and to determine the level of preservatives in PPCPs and to assess the health risk to susceptible populations such as children.

• Journal of Korean Society for Atmospheric Environment
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• v.22 no.2
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• pp.259-266
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• 2006

A dual-channel glass coil sampling technique was used to measure hourly formaldehyde concentration in the ambient air. The dual-channel coil sampling assembly consists of three parts; an all-pyrex 28-turn coil made of 0.2-cm internal diameter glass tubing for gas-liquid contact and scrubbing of soluble gases, an inlet section upstream of the coil for introducing sample air and scrubbing solution, and a widened glass section downstream of the coil for gas-liquid separation. The scrubbing solution used was a dilute aqueous DNPH (dinitrophenylhydrazine) solution. Hourly concentration of formaldehyde was determined at a Gwangju semi-urban site during two intensive studies between September and October using the dual channel glass-coil/DNPH sampling technique and HPLC (High Performance Liquid Chromatography) analysis. The mean concentration was 1.7($0.4{\sim}4.7$) and 3.0($0.5{\sim}19.1$) ppbv for the September and October intensives, respectively, which are considerably low, compared to those measured in polluted urban areas around the world including several urban areas of Korea. The diurnal variation showed significant increase of formaldehyde in the daytime suggesting the dominance of formation of formaldehyde due to photochemical oxidation of methane and other hydrocarbons. An increase in the formaldehyde sometimes in the night might be due to an increase in primary source, i.e. traffic emissions. It was also found that rapid increase in formaldehyde levels from 3.0 to 19.1 ppbv in the afternoon on October 20 was due to plumes from burning of agricultural wastes such as rice straw and stubble. It is expected from the measurement data that the constructed dual-channel glass coil sampling system can be utilized for measuring atmospheric concentration of the formaldehyde with high time resolution.

• Korean Journal of Pharmacognosy
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• v.43 no.4
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• pp.279-285
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• 2012

The Mume Fructus (MF) has been used for relieves cough, arrests arrest chronic diarrhea, treat fluid depletion, and treat ascariasis in Korea. In this study, a high-performance liquid chromatography (HPLC) method was established for simultaneous determination of six main components of MF. Additionally, we were investigated the anti-inflammatory and anti-allergic effects of MF extract on lipopolysaccharide (LPS)-treated RAW264.7 cells and tumor necrosis factor (TNF)-${\alpha}$/interferon (IFN)-${\gamma}$-treated HaCaT cells. The analytical column for separation was used a Gemini $C_{18}$ column maintained at $40^{\circ}C$. The mobile phase consisted of 1.0% (v/v) acetic acid in water (A) and 1.0% (v/v) acetic acid in acetonitrile (B). The flow rate was 1.0 mL/min and the detector was a photodiode array (PDA) set at 280 nm and 320 nm. We evaluated the inhibitory effect of MF extract on the production of inflammatory markers, nitric oxide (NO) and prostaglandin $E_2$ ($PGE_2$) in LPS-stimulated RAW264.7 cells and thymus- and activation-regulated chemokine (TARC/CCL17) in TNF-${\alpha}$/IFN-${\gamma}$-treated HaCaT cells, respectively. We confirmed the genes expression related with TARC, macrophage-derived chemokine (MDC/CCL22) and regulated on activation, normal T cell expressed and secreted (RANTES/CCL5) in HaCaT keratinocyte cells by MF extract. The contents of the five compounds in MF were 0.22-1.01 mg/g. Also, the MF extract show inhibition of about 78% and 75% on NO and $PGE_2$ production at the concentration 1000 mg/mL in RAW264.7 cells. MF extract suppressed the hTARC level and genes expression such as TARC, MDC, and RANTES on TNF-${\alpha}$/IFN-${\gamma}$-treated HaCaT cells.