• 약학회지
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• 제57권5호
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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.

• Journal of Applied Biological Chemistry
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• 제64권1호
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• pp.57-61
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• 2021

Saikosaponin derivatives such as saikosaponins A, B1, B2, B3, B4, C, and D present in Bupleurum falcatum were analyzed by a high performance liquid chromatograph equipped with an evaporative light scattering detector, using different extraction solvents (water and 70% ethanol). The samples were injected into a YMC Pack Pro C18 column and separated using a gradient elution system with a mobile phase composed of acetonitrile and water at a flow rate of 1.1 mL/min. The content of saikosaponin derivatives was higher in 70% ethanol extract than in water extract. This study provides an efficient analytical method for determining the optimal conditions for extraction of saikosaponin derivatives, which can be used as a basis for development of functional foods and pharmaceutical products from B. falcatum.

• 식품기술
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• 제22권1호
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• pp.21-28
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• 2009

• 분석과학
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• 제33권5호
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• pp.209-214
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• 2020

This study has been carried out to develop a standard method for quantifying of 3 permitted artificial sweeteners (including sodium saccharine, aspartame, acesulfame potassium) contained in foods by HPLC-DAD. A simple and rapid sample pretreatment method was used to remove fat and protein from the test solution with Carrez clearing regent precipitant know to be effective for protein and fat removal. The artificial sweeteners in the test solution purified through sample pretreatment were detected by high performance liquid chromatograph using a Reverse phase C18 column (5 ㎛, 4.6 × 250 mm). The simultaneous quantitative test of 3 kinds of artificial sweeteners can be effectively performed on the high fat emulsified foods containing a large amount of fat. Using the established simultaneous quantitative test method, artificial sweeteners were tested in foods such as dairy products, snacks and chocolate. The results calibration curve showed good linearity with high regression coefficients and the result of recovery test showed satisfactory recoveries within 80~110 %.

• 분석과학
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• 제19권6호
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• pp.519-528
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• 2006

본 연구에서는 뇨시료를 고체상 추출법으로 추출한 후 HPLC/DAD/ESI-MS(high-performance liquid chromatograph/diode array detector/electro-spray ionitation mass spectrometry)를 사용하여 분석하였다. 7종의 thyroid hormones의 HPLC 분리조건은 Hypersil ODS(octadecylsilica) 컬럼(4.6mm I.D., 100 mm length, particle size $5{\mu}m$)을 사용하고 ammonium formate buffer와 acetonitrile을 이동상으로 하여 기울기 용리한 결과 완전 분리가 가능하였으며, UV spectra 및 질량스펙트럼을 확인할 수 있었다. 고체상 추출법에 의한 전처리 최적 조건을 조사한 결과 시료를 pH 3으로 한 후 C18 고체상을 사용하여 4 mL의 methanol/ammonium hydroxide(9:1) 혼합용액으로 용리할 경우 회수율이 89.0-113.1%로 나타났다. HPLC/DAD를 이용하여 10-1000 ng/mL범위에서 검량선을 작성한 결과 $r^2$값은 0.992-0.998 으로 나타났으며 검출한계는 2-4 ng/mL(3.8-13.0 pmol/mL)로 계산되었다.

• International Journal of Automotive Technology
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• 제8권1호
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• pp.119-126
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• 2007

Because of the low temperature operation, proton exchange membrane (PEM) fuel cell has a water phase transition. Therefore, water management is an important operation issue in a PEM fuel cell because the liquid water in the fuel cell causes electrode flooding that can lower the cell performance under high current density conditions. In this study, in order to understand the reactant distributions in the cathode channels of the PEM fuel cell, an experimental technique that can measure the species concentrations of reactant gases by using gas chromatograph (GC) is applied for an operating PEM fuel cell. The oxygen distribution along the cathode flow channels of PEM fuel cell is mainly investigated with various operating conditions. Also, the relations between cathode flooding and oxygen concentrations and oxygen consumption pattern along the cathode channel configurations of the unit cell adopted for this study are discussed using GC measurement and visualization experiment of cathode flooding. It is found that the amount of oxygen consumption is very sensitive to various operating conditions of the fuel cell and was much affected by the flooding occurrence in cathode channels.

• 한국환경보건학회지
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• 제19권2호
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• pp.55-60
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• 1993

This study was performed to investigate the effect of washing with water and detergent on the vitamin C content in strawberry and perilla leaf. Vitamin C was extracted with the solution of metaphosphoric acid and quantitated by high performance liquid chromatograph (HPLC). There was no significant difference of vitamin C content between the washing with distilled water and tap water. Three available detergents reduced the vitamin C content of samples to 92.5%, 92.2% and 78.5%, respectively. The content of vitamin C in samples was decreased by increasing the concentration of detergent and washing time.

• Journal of Pharmaceutical Investigation
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• 제14권4호
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• pp.161-169
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• 1984

The tests of dissolution and bioavailability of six formulas of lorazepam tablet under various binders were performed. Lorazepam can be seperated in pharmaceutical preparation and biological plasma by high performance liquid chromatograph. Dissolution process of lorazepam tablet was largely influenced by binder and the dissolution rate was increased by sodium starch glycolate and microcrystalline cellulose, the slower dissolution rate in starch. Bioavailability of lorazepam tablet got relationship with dissolution rate, because tablets containing sodium starch glycolate and microcrystalline cellulose as binder maintained higher plasma level than other binders.

• 분석과학
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• 제26권2호
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• pp.142-153
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• 2013

Milbemycin계 속효성 살충제인 lepimectin의 국내 잔류허용기준이 신설 고시됨에 따라 농산물 중 lepimectin 잔류량을 측정하기 위해 고성능 액체크로마토그래프를 이용한 신속, 정확한 분석법을 개발하였다. Lepimectin 잔류물은 메탄올로 추출하여 포화식염수와 디클로로메탄을 이용한 액액분배를 수행하였고, 플로리실로 충진한 유리칼럼 및 아미노프로필 카트리지를 이용하여 두 번의 정제 과정을 거친 후 HPLC-PAD (High performance liquid chromatograph-photodiode array detector)를 통해 기기분석을 수행하였으며, LC-MS (Liquid Chromatograph-Mass Spectrometer)로 재확인하였다. Lepimectin 표준품의 직선성은 lepimectin $A_3$, $A_4$ 모두에서 상관계수($R^2$)가 0.9999로 우수하였다. 개발한 분석법으로 오이, 고추, 현미, 감귤, 감자, 대두에 대한 lepimectin의 회수율을 측정한 결과, 76.0~114.8% 범위로 10% 미만의 표준오차를 나타내었으며, 분석법의 검출한계는 0.005 mg/kg, 정량한계는 0.01 mg/kg이었다. 또한 광주지방식약청, 대전지방식약청의 분석법 검증 결과, 각각 70.3~108.8%, 80.5~95.6%의 회수율과 10% 미만의 표준 오차를 나타내었다. 분석법에 대한 각 실험실의 회수율과 표준오차 및 실험실간 표준 오차($RSD_R$; Relative Standard Deviation on Reproducibility)는 코덱스 기준(CAC/GL 40)에 적합함을 확인하였다. 따라서 본 연구에서 개발된 분석법은 lepimecin 잔류물의 안전관리를 위한 최적의 분석법으로 판단된다.

• Journal of Biosystems Engineering
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• 제31권5호
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• pp.443-448
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• 2006

For development of an on-line monitoring unit of fermentation process, an auto dilution unit based on traditional chemical and biological analytical method was developed and the performance was evaluated. The dilution unit was constructed with two syringe pumps and flow direction change valves and fully automated. Total delivery volume of two pumps using distilled water was measured to confirm the operating stability And diluted concentrations of three substrate solutions (glucose, lactic acid, ethanol) were compared with a standard method with a high performance liquid chromatograph (glucose, lactic acid) and gas chromatograph (ethanol). Relative error values of total delivery volume of the pumps were below 3% and standard deviation values were 0.003 (n=5). Relative error values of diluted concentration of the dilution unit measurements were below 2% with 1/10 of dilution ratio and 70, $80{\mu}{\ell}$ of sample volume conditions for glucose and lactic acid, 1/30 of dilution ratio and $70{\mu}{\ell}$ of sample volume conditions for ethanol, respectively. In case of the ethanol, cause of the evaporative characteristics, the relative error values showed over 5% whole experimental conditions.