• Journal of Applied Biological Chemistry
• /
• 제43권2호
• /
• pp.94-100
• /
• 2000

An analytical method was developed to determine abamectin and milbemectin residues in apple, pear, and citrus using HPLC with ultraviolet absorption detection. Abamectin and milbemectin were extracted with methanol from apple, pear, and citrus samples. The extract was diluted with saline water and dichloromethane partition was followed to recover the compounds from the aqueous phase. Florisil column chromatography and aminopropyl solid-phase extraction were employed as cleanup methods to remove most of co-extractives from the sample extract. Reverse-phase HPLC using an octadecylsilyl column was successfully applied to separate and quantitate abamectin and milbemectin residues in sample extracts at the wavelength of 245 nm. Recoveries of abamectin and milbemectin from fortified samples ranged 80.4~90.3% and 90.9~96.8%, respectively. Relative standard deviations of the analytical method were less than 10% for both acaricides. Detection limit of the analytical method was 0.003 mg/kg sample for all the analytes. The proposed method was reproducible and sensitive enough to evaluate terminal residues of abamectin and milbemectin in apple, pear, and citrus.

• 분석과학
• /
• 제10권6호
• /
• pp.445-452
• /
• 1997

뇨 중에 Putrescine, Spermidine 및 Spermine benzoyl chloride를 유도체화제로 처리한 다음 HPLC법으로 정량하였다. ${\mu}$-Bondapak $C_{18}$ 컬럼과 methanol/$H_2O$(50/50v/v)를 사용하여 정상인 및 자궁암 환자의 뇨 중에서 Putrescine, Spermidine 및 Spermine을 역상법으로 분석한 결과 암환자의 경우 정상인에 비해 이들 polyamine이 현저한 증가를 보였다.

• 미생물학회지
• /
• 제30권2호
• /
• pp.96-100
• /
• 1992

토양세균의 혼합배양에 의한 MCPP [2-(2-Methyl-4-Chlorophenoxy) Propionic Acid]의 미생물학적 분해를 조사하였다. 혼합배양은 Pseudomonas 종, Flavobacterium 종, 그리고 Achromobacter종을 포함하였다. 세균들은 유일한 탄소 및 에너지원으로서 MCPP를 이용하였으나, 부분적인 분해만을 부여주었다. MCPP의 분해는 2-methyl-4-chlorophenol의 형성에 의하여 진행되었으며, 이는 HPLC 에 의하여 발견되었고, GC-MS에 의하여 확인되었다. 이 중간대사물질은 일시적으로 생성되었으며, reverse phase HPLC와 Uv absorbance에 의하여 다른 대사산물의 존재는 관찰되지 않았다.

• Biomolecules & Therapeutics
• /
• 제16권2호
• /
• pp.168-172
• /
• 2008

The present study is to determine of sensitive nicorandil analysis method using HPLC and measure the pharmacokinetics parameters (bioavailability, $C_{max}$, $T_{max}$, Ke, $T_{1/2}$) of nicorandil (5 mg, Tab; Choongwae Pharma Corporation). Plasma (500 ul) was mixed with furosemide (internal standard, 500 ug/ml). Detection wavelength was 256 nm. The mixture of 0.01 M ammonium acetate and acetonitrile 80:20 (v/v) was used mobile phase. The HPLC separation was accomplished on ODC reverse HPLC column. The nicorandil was analyzed by a HPLC system, which consists of CAPCELL PAK C18 column (5 ${\mu}$m, 4.6 × 150 mm) and a chromatography data analysis S/W, using a isocratic mobile phase (mixture of 0.01 M ammonium acetate and acetonitrile 80:20 ) at 1.0 ml/min. Its sensitivity, selectivity, accuracy and precision must be adequate for the bioavailabilty study of nicorandil, and the linearity ($r^2$ ≥ 0.9994) of nicorandil was also proved in the range of 0.05 ug/ml . 3 ug/ml. The pharmacokinetic parameters of nicorandil (5 mg) tablets were measured as the follow. AUC: 0.19 ug/ml·hr, $C_{max}$: 0.14 ug/ml, $t_{max}$: 0.58 hr, Ke: 0.11 hr., $t_{1/2\beta}$: 6.76 hrs. This method is simple and sensitive HPLC method using UV detector for determination of nicorandil in human plasma.

• 약학회지
• /
• 제54권4호
• /
• pp.316-321
• /
• 2010

Adefovir dipivoxil which was originally developed by Gilead Sciences has been used as treatments of HIV and HBV, especially a therapeutics for HBeAg positive and negative chronic patients. We developed highly efficient purification method using reverse phase column chromatography for mass production and a stable amorphous Adefovir dipivoxil using solid dispersion method. Reverse phase column chromatography led to highly pure product, more than 99.7% by HPLC and can be used for mass production compared with normal column chromatography. Solid dispersion method containing watersoluble polymer and Isomalt showed improved stability of amorphous Adefovir dipivoxil against heat and moisture.

• Applied Biological Chemistry
• /
• 제33권4호
• /
• pp.307-314
• /
• 1990

Brassinosteroid는 특이한 생리작용을 갖는 식물의 신 생장조절물질로 주목을 받고 있으나, 아직 우리나라의 가장 중요한 작물인 벼의 brassinosteroid에 대해 연구된 바 없어, 일반계 품종의 벼를 대상으로 brassinosteroid활성물질의 검색을 시도하였다. 동진벼와 영산벼를 최고분얼기까지 재배하여 지상부를 수확하고, 유기용매로 추출하여 얻어진 추출물에서 rice lamina inclination test에 의한 생물검정법으로 활성이 인정되어, 활성본체의 구명과 정제의 목적으로 각각의 활성획분을 silica gel 흡착 chromatography, Sephadex LH-20 chromatography, charcoal 흡착 chromatography, preparative TLC, Bondesil chromatography 그리고 normal, reverse phase의 HPLC 등적 방법으로 분획하여 검정한 결과 2품종 모두 brassinosteroid활성물질을 생산하고 있으며, 또 2품종간의 endogenous brassinosteroid의 유사성이 인정되었다.

• 대한한의학방제학회지
• /
• 제18권2호
• /
• pp.251-257
• /
• 2010

Objectives : To develop and validate High-performance liquid chromatography-photodiode array methods for simultaneous determination of two constituents in Oryeong-san(ORS). Methods : Reverse-phase chromatography using a Gemini C18 column operating at $40^{\circ}C$, and photodiode array(PDA) detection at 280 nm, were used for quantification of the two marker components of ORS. The mobile phase using a gradient flow consisted of two solvent systems. Solvent A was $H_2O$ and solvent B was acetonitrile. Results : Calibration curves were acquired with correlation coefficient ($r^2$)>0.9999, and the relative standard deviation(RSD) values(%) for intra- and inter-day precision were not exceed 1.0%. The recovery rate of each compound was in the range of 93.01-104.16%, with an RSD less than 2.0%. The contents of two compounds in ORS were 1.10-3.72 mg/g. Conclusions : The established HPLC method will be helpful to improve quality control of ORS.

• Natural Product Sciences
• /
• 제13권2호
• /
• pp.148-151
• /
• 2007

High performance liquid chromatography (HPLC) was used for the analysis of chiisanoside in Acanthopanax species. A reverse-phase system using a gradient of H$_2$O and acetonitrile as the mobile phase was developed and a wavelength of detection was at 210 nm. The analysis was successfully carried out for 30 min. Chiisanoside was measured in the fruit, stem and root of A. sessiliflorus, A. koreanus, A. divaricatus and A. senticosus.

• 약학회지
• /
• 제50권1호
• /
• pp.21-25
• /
• 2006

Reiterated normal-phase column chromatography lead to the isolation and purification of six known compounds but for the first time from the whole plant of Sasa borealis (Hack.) Makino (Gramineae): tricin 4'-O-(erythro-${\beta}$-guaia-cylglyceryl) ether (1), tricin 4'-O-(threo-${\beta}$-guaiacylglyceryl) ether (2), tricin 4'-O-[erythro-${\beta}$-guaiacyl-(9'-O-acetyl)-glyceryl] ether (3), tricin 4'-O-[threo-${\beta}$-guaiacyl-(9'-O-acetyl)-glyceryl] ether (4), (-)-pinoresinol (5), and vanillin (6). The structures of the compounds (1-6) were established based on interpretation of high resolution NMR (COSY, HSQC, HMBC, and NOESY) spectral data. In particular, compounds 1 and 3 were diastereomers of compounds 2 and 4, respectively. These two sets of diastereomers were able to be simultaneously identified and quantified by a gradient reversed-phase HPLC method with UV photodiode array, This sensitive HPLC method is noteworthy as a simultaneous separation and identification method to test the extract of the family Gramineae which contains these compounds.

• Applied Biological Chemistry
• /
• 제41권8호
• /
• pp.595-599
• /
• 1998

An analytical method was developed to determine tricyclazole residues in rice grain, straw, and soil using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. Tricyclazole was extracted with methanol from moist rice grain, straw, and soil samples. n-Hexane washing was employed to remove nonpolar co-extractives during liquid-liquid partition. Tricyclazole was then extracted with dichloromethane from alkaline aqueous phase, while acidic interferences remained in the phase. Dichloromethane extract was further purified by silica gel column chromatography prior to HPLC determination. Reverse-phase HPLC using an octadecylsilyl column was successfully applied to separate and quantitate the tricyclazole residue in sample extracts monitored at ${\lambda}_{max}$ 225nm. Recoveries from fortified samples averaged $95.5{\pm}3.0%\;(n=6),\;87.5{\pm}20.%\;(n=6),\;and\;84.3{\pm}2.8%$ (n=12) for rice grain, straw, and soil, respectively. Detection limit of the method was 0.02 mg/kg for rice grain and soil samples while 0.05 mg/kg for rice straw samples. The proposed method was reproducible and sensitive enough to evaluate the safety of tricyclazole residues in rice grain, straw, and soil.