• YAKHAK HOEJI
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• v.57 no.5
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• pp.362-368
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• 2013

High performance liquid chromatograph (HPLC) is the most frequently used analytical instrument in analytical laboratories for pharmaceutical analysis. In order to provide a high level of assurance for reliable data generated from the HPLC analysis, the performance qualification of the HPLC system is required. For this purpose, the performance of HPLC system should be regularly monitored by examining the key functions of the typical HPLC system (solvent delivery system, injector system, column oven, UV-VIS detector system). We have investigated the validation guidelines of the performance verification of these key modules for HPLC system. And we proposed and evaluated its validation guidelines and the related verification methods for pharmaceutical analysis that could be practically applied in Korea.

• Korean Journal of Food Science and Technology
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• v.35 no.6
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• pp.1028-1032
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• 2003

To assess accurate methods for measuring sulfur dioxide residue in pickles, the acid distillation HPLC-UV method and Monnier Willams modified method were examined. By the acid distillation HPLC-UV method, sulfites released from pickles by acid distillation were absorbed in 1% triethanolamine solution and detected as sulfite ion by HPLC with UV monitoring at 240nm. An anion exchange column was employed with 1.8mM $Ma_2CO_3-1.7mM\;NaHCO_3$ solution as a mobile phase, $84.0{\sim}91.7%$ of sulfite added to pickled radish were recovered. Total sulfite levels from 48 kinds of pickles analyzed by acid distillation HPLC-UV was compared with those analyzed by the Monnier Williams modified method. The Monnier Williams modified method showed higher levels of sulfur dioxide than the acid distillation HPLC-UV method due to the presence of volatile acids in pickles. The concentration of sulfur dioxide was in the range of $N.D{\sim}173.05ppm$ in pickled radish and over 30ppm of sulfur dioxide from 3 samples by the acid distillation-HPLC-UV method.

• Korean Journal of Medicinal Crop Science
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• v.10 no.3
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• pp.200-205
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• 2002

Platycodin D was isolated from n-butanol extract of Platycodi radix(Platycodon grandiflorum and identified by the spectroscopic analysis using $^1H$ and $^{13}C$ NMR techniques. A new method of analysis of platycodin D by high performance liquid chromatography(HPLC) was established using a reversed phase system with YMC-Pack ODS-AM( 250 X 4.6 mm) column and 30% acetonitrile as a mobile phase. Evaporative light scattering detector was used as detector. The kinds of extraction solvents and methods were examined to determine the efficient extraction condition and HPLC analysis was carried out to establish the optimum drying condition for the root of Platycodon grandiflorum. The contents of Platycodin D was highest as 0.083% when platycodon roots were dried at $60^{\circ}C$ using dry oven.

• Korean Journal of Food Science and Technology
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• v.32 no.6
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• pp.1437-1441
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• 2000

Acycloretinoic acid was prepared from acycloretinal by oxidation with Tollens reagent. Acycloretinoic acid was separated with Silica-HPLC and analyzed by ODS-HPLC with a photodiode array detector and by GC-MS. Lycopene was solubilized in toluene and aqueous Tween 40, and then oxidized by incubating at $37^{\circ}C$ under atmospheric oxygen. Acidic compound was produced by autoxidation of lycopene. Retention time, UV-Vis spectra and mass spectra of the acidic compound were identical to the standard acycloretinoic acid. Thus, acycloretinoic acid was confirmed to occur in vitro under oxidation condition of lycopene.

• Journal of environmental and Sanitary engineering
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• v.7 no.1
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• pp.79-86
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• 1992

Rapid determination of chlorpyrifos and fluvalinate in mixed insecticide was established by using high performance liquid chromatography. Result were as follows : 1. On Lichrosorb${\circledR}$ RP-8(10 ${\mu}m$) Column with on fluent of acetanitrile : water=75 . 25, sufficient separation of Chlorpyrifos and Fluorinate of base was obtained. 2.410td portion the diluted solution was injected in to the cdumn, and the effluent was monitored by on UV-Detector at 270 nm. 3. Relative Standard Deviation were 0.97% (chlorpyrifos) and 0.5% (fluorinate) under analysis conditions. 4. The UV-Detector response at 270 nm were linear (Y=421.8X-2090, $R^2=0.9997$ : Chlorpyrifos, Y= 1062.7X-4017.7, $R^2=0.9998$ : Fluorinate) over a range of 30~500 ${\mu}g/ml$.

• Journal of the Korean Society of Food Science and Nutrition
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• v.29 no.4
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• pp.568-574
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• 2000

Phytofluene was subjected to ozonolysis in ice-cold dichloromethane. The ozonolysis products were fractionated with a silica column and the carbonyl fraction was analyzed by ODS-HPLC with a photodiode array detector. Phytofluene was solubilized in 5% tween 40, and then oxidized by incubating under dim yellow light at 37$^{\circ}C$, 24 hr with continuous shaking. Carbonyl compound and acidic compound were produced. In comparison with autoxidation and ozonolysis, each compound showed the same retention time and UV-vis spectra were identical to the reference cleavage products prepared by ozeonolysis of phytofluene. Absorption spectrum of acidic compound was similar to that of standard 4,5-didehydrogeranyl geranyl acid which is known to possess biological activity. Thus, eccentric cleavage of phytofluene was confirmed to occur in vitro under oxidation condition.

• Natural Product Sciences
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• v.16 no.3
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• pp.164-168
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• 2010

High-performance liquid chromatographic method with diode-array detector and electrospray ionization with multi-stage tandem mass spectroscopy (HPLC/DAD/ESI-$MS^n$) was used to identify the major constituents in a methanolic extract of Eclipta prostrata. The chromatographic separation was performed on a C18 column. Acetonitrile-water was used as a mobile phase. HPLC/DAD/ESI-$MS^n$ allowed the characterization of constituents of E. prostrata, mainly triterpenoids (eclalbasaponin I, II, III, IV, VI), flavonoids (luteolin 7-O-glucoside, demethylwedelolactone, wedelolactone, luteolin, demetylwedelolactone sulfate, luteolin sulfate, apigenin sulfate) and phenolic acids (5-O-caffeoylquinic acid, 3, 4-O-dicaffeoylquinic acid, 3, 5-O-dicaffeoylquinic acid, 4, 5-Odicaffeoylquinic acid).

• Korean Journal of Veterinary Service
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• v.26 no.2
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• pp.145-149
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• 2003

To explore the most sensitive and useful method for simultaneous determination of 8 carbamate pesticides in livestock productions, the mixture of 8 carbonates was determined by HPLC with scanning fluorescence detector. For mobile phase water, acetonitrile and methanol program gradient showed more applicable sensitivity than water and acetonitrile program gradient used ExW 339 nm and EmW 445 nm for fluorescence detector. On using carbamate columns, the retention time was within 4 to 20 minutes. And this made it possible to separate and detect simultaneously. therefore we could analyze it exactly and efficiently and reduce time. The preparation process of MSPD method showed that the high recovery rate was more than 88.5% in most of the carbamate pesticides. Therefore we could say that it was an efficient and fast method analyzing out of lots of samples.

• Bulletin of the Korean Chemical Society
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• v.26 no.10
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• pp.1533-1538
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• 2005

We have determined the contents of monosaccharides in the hydrolysates of some yogurt and orange juice products by derivatizing monosaccharides with p-aminobenzoic acid ethyl ester (ABEE). The separation of the ABEE-derivatized monosaccharides was efficiently carried out by HPLC using a microcolumn packed with the Alltima $C_{18}$ stationary phase. The concentrations of monosaccharides were determined based on the measured peak area/height counts. ABEE derivatization of fructose and its detection have never been successfully carried out before this work. In this study, two peaks were observed in a fixed ratio for ABEE-fructose, and the ratio was maintained over a wide range of fructose concentration. In order to prove the validity of the above method, we compared the concentrations of glucose, galactose and fructose determined by ABEE derivatization and UVD (ultraviolet detector) chromatography with those determined by RID (refractive index detector) chromatography without derivatization. The determined concentrations of monosaccharides obtained from the two chromatographic methods were found close to each other within acceptable error ranges.

• Korean Journal of Food Science and Technology
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• v.32 no.6
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• pp.1227-1233
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• 2000

Lycopene was subjected to ozonolysis in ice-cold dichloromethane. The ozonolysis products were fractionated with a silica column and the carbonyl fraction was analyzed by ODS-HPLC with a photodiode array detector and by LC-MS. UV-vis spectra and $[M+H]^+$ of the carbonyl compound peaks showed clearly that acycloretinal, apo-14'-lycopenal, apo-12'-lycopenal, apo-10'-lycopenal, apo-8'-lycopenal and apo-6'-lycopenal were formed by ozonolysis of lycopene. Lycopene was solubilized in toluene and aqueous Tween 40, and then oxidized by incubating at $37^{\circ}C$ under atmospheric oxygen. Carbonyl compounds were produced. In comparison with autoxidation and ozonolysis, each compound showed the same retention time and UV-vis spectra are identical to the reference cleavage products prepared by ozonolysis of lycopene. Thus, eccentric cleavage of lycopene was confirmed to occur in vitro under oxidation condition.