• Journal of Pharmaceutical Investigation
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• 제35권6호
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• pp.461-465
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• 2005

A simple HPLC method with ultraviolet detection of nicardipine in human plasma was developed and validated. After drug extraction with solid phase extraction (SPE) method, chromatographic separation of nicardipine in plasma was achieved at $30^{\circ}C$ with a $C_{18}$ column and acetonitrile-0.02% phosphate buffer mixture (with 0.02% triethylamine, final pH 7.0), as mobile phase. Quantitative determination was performed by ultraviolet detection at 254 nm. The method was specific and validated with a limit of quantification of 5 ng/mL. The intra- and inter-day precision and accuracy were acceptable for all quality control samples including the lower limit of quantification. The applicability of the method was demonstrated by analysis of plasma after oral administration of a single 40 mg dose to 8 healthy subjects. From the plasma nicardipine concentration versus time curves, the mean $AUC_{t}$, was $134.04{\pm}59.72\;ng\;hr/mL$ and $C_{max}$ of $108.65{\pm}69.17\;ng/mL$ reached 1.5 hr after administration. The mean biological half-life of nicardipine was $3.93{\pm}0.82\;hr$. Based on the results, this simple and validated assay method could readily be used in any pharmacokinetic or bioequivalence studies using human.

• 대한본초학회지
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• 제30권4호
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• pp.11-20
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• 2015

Objectives : Ongyeong-tang (OGT) is a traditional herbal formula used to cure gynaecological disorders. OGT consists of 12 herbal medicines containing various bioactive components. Therefore, the development of suitable analytical method for the marker compounds is necessary for the quality control of OGT. Methods : Determination of the 18 marker compounds in OGT preparations was quantitatively performed by high-performance liquid chromatography-photodiode array detection analysis. The marker compounds were separated on a reversed-phase C ₁₈ column and the analytical method was successfully validated, which was applied to compare OGT extracts from laboratory preparation and commercial OGT granules. Results : Limit of detection and limit of quantification values were in the ranges of $0.001-0.016{\mu}g/mL$ and $0.003-0.047{\mu}g/mL$, respectively. Precision was 0.03-3.71 % within a day and 0.03-3.81 % over four consecutive days. Recovery of marker compounds ranged from 90.63-108.26 %, with relative standard deviation (RSD) values < 4.0 %. Reproducibility was < 2.5 % of the RSD value. The 18 marker compounds were stable within 16 h at $10^{\circ}C$, with the RSD value < 3.5 %. Quantitative analysis results showed that the quantities of the 18 marker compounds varied among OGT samples. Pearson coefficient evaluation and principal component analysis demonstrated that an OGT water extract produced by a laboratory method clearly differed from commercial OGT granules. Conclusions : The developed analytical method was simple, precise, and reliable. Therefore, it can be used for the quality assessment of OGT preparations.

• 한국수산과학회지
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• 제38권6호
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• pp.372-378
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• 2005

An analysis method of tetracyclines far fish and shellfish products containing large amount of low molecular materials and pigments was established. The recovery of the established analysis method for four tetracycline samples was $72-100\%$ and higher than other methods reported. Especially, proposed sample treatment protocol was shown to be effective for the removal of low molecular materials and pigments that tend to interfere with accurate analysis. The detection limit of oxytetracycline (OTC) and tetracycline (TC) from the sample was 0.02 ppm, and the detection limit of chlortetracycline (CTC) and doxycycline (DC) from the sample was 0.1ppm, To examine the efficiency of the established method and identify tetracycline usage in fish farms, tetracycline group antibiotics in the flounder being cultured was monitored. The improved method can be used for fish and shellfish products effectively and all surveyed fish farms have used tetracycline all the year round. The proposed method was adopted as official method for fishery products by Korean Food and Drug Administration in 2003 and it is being used by regulatory authority as National Fishery Products Quality Inspection Service.

• 한국식품영양학회지
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• 제32권2호
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• pp.148-154
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• 2019

The aim of this study was to select compounds for the standardization of fermented Kalopanax pictus Nakai (KP-F), to develop the analysis method using HPLC-PDA and to perform method validation. KP-F is a fermented powder developed to improve the original physiological activities and create a new functionality. Eleutheroside E, Acanthoside B, and Syringaresinol were selected as the standard compounds and developed our own method for simultaneous analysis. The analyte was isolated using C18 column with a gradient elution of 0.05 M phosphoric acid in water and methanol as the mobile phase at a flow rate of 1 mL/min and detected at 210 nm. As a result, all standard compounds showed good linearity with an $R^2$ (coefficient of correlation) of 1.000 and for the limit of detection range of $0.710{\sim}0.831{\mu}g/mL$, and the limit of quantification as $2.150{\sim}2.520{\mu}g/mL$. The precision was RSD (%) of less than 4.80%, while the accuracy was 4.70%>RSD (%) for the range 102.44~110.48%. In conclusion, the developed analysis method is suitable for the detection of Eleutheroside E, Acanthoside B, and Syringaresinol in KP-F.

• 한국산업보건학회지
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• 제7권2호
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• pp.223-232
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• 1997

The accuracy and precision of a modified method of NIOSH Method 7600 and EPA method 218.6 was determined for analyzing hexavalent chromium, Cr(VI), collected on PVC filter from workplace air. The method was designed to extract from Cr(VI) on PVC filter with a alkali solution, 2% NaOH/3% $Na_2CO_3$, and to analyze it using ion chromatography/visible absorbance detection(IC/VAD). The results and conclusion are as the following. 1. The peak of Cr(VI) was separated sharply on chromatogram and was linearly related with Cr(VI) concentration in sloution. The correlation coefficient was 0.9999 in a calibration curve. The limit of detection was 0.25 $0.25{\mu}g/sample$. 2. The accuracy(% recovery) was 93.3% in a set of sample($9-50{\mu}g$) stored for a day, and 100.1%($10-60{\mu}g$) in another set of samples stored for 2 hours. It is assumed that the difference in recovery by storage time was due to reduction of Cr(VI) to Cr(III). 3. The precision(coefficient of variation, CV) of the method was 0.015 in spiked samples with Cr(VI) standard solution, and 0.010 in spiked samples with plating solution from a chrome electroplating factory. The overall CV in all types of samples was 0.0013. 4. The Cr(VI) was stable in 2% NaOH/3% $Na_2CO_3$ at least for 10 hours. In conclusion, the IC/VAD method is appropriate for determining low-level Cr(VI) in workplace air containing various interferences.

• 분석과학
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• 제27권1호
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• pp.60-65
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• 2014

전통주류의 한가지인 막걸리 중의 기능성 성분인 E,E-farnesol과 squalene를 분석하는 방법을 확립하였다. 막걸리에 들어있는 E,E-farnesol과 squalene은 stir bar sorptive extraction (SBSE)와 GC-MS를 사용 분석하였다. SBSE방법은 막걸리 중의 E,E-farnesol과 squalene함량을 분석하는데 매우 효율적이었다. 이 두 성분을 SBSE법으로 분석하였을 때 E,E-farnesol은 0.5-200 ng/mL ($R^2=0.9974$) 범위에서 squalene은 100-50000 ng/mL ($R^2=0.9982$)에서 직선성을 보였다. SBSE법으로 분석할 경우 E,E-farnesol과 squalene의 limit of detection (LOD)와 limit of quantification (LOQ)는 각각 0.1 과 0.5 ng/mL 및 15.0과 40.0 ng/mL 이었다. SBSE법에 의한 E,E-farnesol과 squalene의 회수율은 각각101-107%와 98-103%로 정확도가 매우 높았다.

• 분석과학
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• 제23권6호
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• pp.587-594
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• 2010

완제품의 주성분인 옥시라세탐이 함유된 의약품의 시험법실시 계획서에 따른 시험이 적절히 진행되었는지 시험법의 검증여부를 하고 본 protocol이 완제품 중 옥시라세탐의 정량분석을 위한 HPLC 분석법의 타당성을 검증하기 위한 문서화된 절차를 제공하는 것을 목적으로 한다. 본 실험에서는 옥시라세탐 함량시험에 사용된 분석법에 대하여 시스템 적합성, 정밀성, 직선성, 범위, 정확도, 특이성, 정량한계, 검출한계에 대하여 확인하였다. 실험결과 시스템적합성에서 정밀도(RSD%) 0.127%이하, 이론단수 15081, tailing factor 0.49, 그리고 분리능 32.41을 나타내었고, 정밀도실험에서는 RSD% 0.359% 이하의 결과를 보였다. 그리고 직선성 실험에서는 상관계수($R^2$)가 1을 나타내었고, 정확도 실험에서는 recovery test로서 최소 98.4%, 최대 99.6%로 기준을 만족하였다. 검출한계는 0.1 mg/L이였으며, 정량한계는 0.5 mg/L이었다. 그리고 특이성 실험에 있어서도 기준을 만족하는 결과를 나타내어 옥시라세탐을 주성분으로 하는 완제의약품 시험법은 적합한 시험법임이 검증되었다.

• 대한화장품학회지
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• 제49권4호
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• pp.291-298
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• 2023

본 연구에서는, 화장품 중 로션, 크림, 클렌저 제형에 적용된 세라마이드엔피(ceramide NP)의 함량을 분석하고자 high-performance liquid chromatography (HPLC)를 이용한 정량 분석 방법을 개발하였다. 분석은 C18 칼럼을 이용하고 이동상은 아세토니트릴과 메탄올을 70 : 30 비율로, 유속은 0.8 mL/min으로 하고 칼럼 온도는 20 ℃로 조건을 설정하였다. 분석 방법은 ICH 가이드라인에 따라 특이성, 직선성, 검출한계(LOD) 및 정량한계(LOQ), 정확성, 정밀성을 분석하여 검증하였다. 분석 방법의 유효성 검증 결과, 검량선의 직선성(R²)은 0.99984로 우수한 직선성을 보였다. 로션, 크림, 클렌저 제형에 대한 정확성은 95.11 ~ 100.48%의 회수율을 통해 확인하였고, 정밀성 분석 결과 상대 표준 편차(RSD)는 0.26% 이하로 나타났다. 검출한계는 0.902 ㎍/mL, 정량한계는 2.733 ㎍/mL로 확인되었다. 이를 통해, 화장품에 적용된 세라마이드엔피의 정량 분석 시, 방해 물질의 영향으로 인해 주피크 분리가 어려운 경우 측정이 가능하게 하여 제품의 품질관리에 도움이 될 것으로 기대된다.

• 대한수의학회지
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• 제45권2호
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• pp.191-197
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• 2005

An immunochromatographic (IC) strip for the rapid detection of Salmonella spp. in the enriched sample was developed. Affinity purified Salmonella polyclonal antibody was conjugated with 40 nm colloidal gold particles which were prepared by citrate method in our laboratory. The antigen-antibody-gold complex was captured by Salmonella antibody attached to test line of nitrocellulose membrane during the capillary migration of sample. Specificity of the IC strip was calculated to be 100% (12/12) and sensitivity was 97.6% (41/42) in the test with pure cultured bacteria. Salmonella was artificially inoculated into raw pork macerated with enrichment broth. And then it was 10-fold diluted from $5.2{\times}10^{8}CFU/ml$ to 5.2 CFU/ml. The IC strip could detect $5.2{\times}10^{6}CFU/ml$ before enrichment. However, the lowest limit of detection was 5.2 CFU/ml after overnight incubation. The results indicated that the IC assay was a rapid, economical and simple method with high specificity and sensitivity for the detection of Salmonella spp. without using any equipment.

• Bulletin of the Korean Chemical Society
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• 제25권6호
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• pp.900-906
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• 2004

An RPLC-postcolumn detection method has been developed for the fluorimetric determination of dichloroacetamide (DCAD) in water. After ammonia and DCAD were separated on a $C_{18}$ nonpolar stationary phase with 2.5% methanol-0.02 M phosphate buffer at pH 3, the column eluant was reacted with post column reagents, o-phthaldialdehyde (OPA) and sulfite ion at pH 11.5, to produce a highly fluorescent isoindole fluorophore, which was measured with a fluorescence detector ( ${\lambda}_{ex}$ = 363 nm, ${\lambda}_{em}$ = 425 nm). With the optimized conditions for RPLC and the postcolumn derivatization, the calibration curve was found to be linear in the concentration ranges of 0.5 and 20 ${\mu}$M for DCAD, and the detection limit for DCAD was 0.18 ${\mu}$M (23${\mu}$g/L). This corresponded to 18 pmol per 100 ${\mu}$L injection volume for a signal-to-noise ratio of 3, and the repeatability and reproducibility of this method were 1.0% and 2.5% for five replicate analyzes of 2 ${\mu}$M DCAD, respectively. The degradation yields DCAD to ammonia were 94 and 99%, and the percent recoveries of DCAD from 4 and 6 ${\mu}$M DCAD-spiked tap water were shown mean more than 97%.