• YAKHAK HOEJI
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• v.57 no.2
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• pp.87-94
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• 2013

An analytical methodology based on solid-space extraction (SPE) with with Bond Elut Certify cartridge (Varian, 130 mg) has been developed for the qualification and quantitation of strychnine in blood. After the elution layer was evaporated, the residue was reconstituted with methanol for GC/MS. Internal standard was used 10 mg/l dextromethorphan. Strychnine is a potent central nervous stimulant and convulsant, and an alkaloid found in seeds of Strychnos nux-vomica. It was used therapeutically to improve circulation and muscle tone in oral or intramuscular doses of 0.05~8 mg. The fatal dose of strychnine for humans is 50~100 mg. A man was found dead lying curled up the corner of the large room in a roof house after the fire fighter opened a locked door inside to put out the fire. The postmortem blood and gastric contents were analyzed for toxicological testing. Strychnine and brucine were detected using GC/MS first in gastric contents extracts. The contents of strychnine was 0.083 mg/l in heart blood, 0.088 mg/l in peripheral blood and 4.0 mg/kg in gastric contents, respectively. Method validation was carried out in terms of linearity, accuracy, precision (intraday, interday) in blood. The assay is linear over 0.05~10 mg/l ($r^2$=0.999). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.02 mg/l (S/N=3) and 0.07 mg/l (S/N=10), respectively. Accuracy (bias%) of strychnine with 0.1, 1 and 10 mg/l was 12.0% (n=6), 9.3% (n=6) and 6.9% (n=6), respectively. Intraday precision (CV%) of strychnine with, 0.1, 1 and 10 mg/l were 6.4%, 10.4%, 1.2% (n=6), respectively. Interday precision (CV%) of strychnine with 0.1, 1 and 10 mg/l over three days were 24.0%, 18.5%, 13.8% (n=18), respectively. Relative recovery with 0.1, 1 and 10 mg/l (in blood) were 114.9%, 99.3% and 87.4% (n=6), respectively. The described method can be applied in forensic toxicology to determine strychnine in blood samples.

• Journal of Dairy Science and Biotechnology
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• v.34 no.3
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• pp.187-191
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• 2016

Biogenic amines have been used as chemical indicators of fermented foods. So far, several chromatography methods have been developed to detect biogenic amines in foods. However, few methods have identified these compound in domestic cheese. We analyzed the biogenic amines (histamine dihydrochloride, tyramine hydrochloride, ${\beta}$-phenylethylamine hydrochloride, putrescine dihydrochloride, cadaverine, spermidine, tryptamine hydrochloride, ethanolamine hydrochloride and butylamine) in cheese by using HPLC. The calibration curves of the biogenic amines were found to be linear over the concentration range of 10-50 ppm with a correlation coefficient of above 0.99. The limit of detection (LOD) and limit of quantitation (LOQ) of the biogenic amines in the given order were 3.7 and 11.3 ppm, 3.4 and 10.4ppm, 3.4 and 10.3 ppm, 4.0 and 12.2 ppm, 3.4 and 10.4 ppm, 3.4 and 10.5 ppm, 3.5 and 10.7 ppm, 4.1 and 12.5 ppm, and 3.4 and 10.4 ppm, respectively. Recovery rates of the biogenic amines in the given order were 112, 104, 93, 108, 91, 102, 101, and 92%, respectively. The findings of this study suggest that HPLC is a suitable method for the determination of biogenic amines, thereby indicating its potential application in the quality control of aging cheese.

• Analytical Science and Technology
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• v.16 no.1
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• pp.32-38
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• 2003

The rapid and sensitive determination method of sildenafil and its related compounds (Vardenafil, Homosildenafil, Tadanafil.) has been investigated using high performance thin layer choromatography (HPTLC). Optimizing separation conditions and simultaneous determination method of these compounds were studied. The calibration curves of those compounds at 254 nm was found to be linear in the range of $1.0{\sim}56.5{\mu}g/mL$, respectively. The detection limts (LOD) and quantification limits (LOQ) of these were found to be $0.8{\sim}1.8{\mu}g/mL$ and $1.0{\sim}2.3{\mu}g/mL$. The coefficient of variation (C.V.) were less than 2.5%. Finally, the present method was applied to determine sildenafil and its related substances in dietary supplement.

• Analytical Science and Technology
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• v.29 no.4
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• pp.202-208
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• 2016

본 연구에서는 사료 첨가제로 이용되고 있는 유기산 7종(formic acid, malic acid, lactic acid, acetic acid, citric acid, fumaric acid, propionic acid)의 동시분석법 개발을 위한 연구를 실시하였다. 7종의 화합물은 표준물질의 Retention time과 UV spectra를 통해 구별하였고, 분석법 검증은 직선성, 민감성, 선택성, 정확성, 정밀성을 통하여 검증하였다. 그 결과로 LOD와 LOQ의 범위가 각각 43~26,755 μg/kg, 12-8,026 μg/kg으로 설정하였고, 평균 회수율이 79.3~95.2%로 우수하게 보였으며, intra-day, inter-day에 대한 전반적인 상대 표준 편차(%RSD)는 3.2% 미만으로 나타났다. 이와 같이 검증된 자료를 통해 유기산의 동시분석에 대한 직선성, 민감성, 선택성, 정확성 및 정밀성을 확인하였고, 높은 수준을 나타냄을 알 수 있었다. 이를 바탕으로 유기산이 검출되는 단미사료 46 가지를 분석에 적용하여 진행하였고, 정량과 동시분석 검출을 위한 방법은 RP-HPLC/UV 검출기를 이용하여 성공적으로 개발되었다. 따라서 본 연구결과를 바탕으로 하여 사료 중의 유기산의 분석이 신속하고 정확해졌을 뿐 아니라, 다른 종류의 사료 또한 이를 적용하여 효율적으로 이용할 수 있을 것으로 판단된다.

• Journal of the Korean Institute of Gas
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• v.13 no.6
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• pp.34-38
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• 2009

Nitrous oxide, which is used as an anesthetic gas, has been shown to be a chronic health hazard. It is necessary to monitor and control the nitrous oxide exposure of the operating theaters staff. In this study, N2O exposure level of the operating nurses is assessed with a GC-ECD. The nitrous oxide gas is collected on a molecular sieve 5A contained in a glass tube and desorbed for 12 hours at $100^{\circ}C$ in heating block. As a result of the test using GC-ECD, calibration curve's $R^2$ of $N_2O$ is 0.9992, LOD is $0.96{\mu}g$/injection, LOQ is $3.21{\mu}g$/injection, desorption efficiency is 94.78 4.50% in average and break through is within 10% compared with the concentration. The average concentration before operation is 5.12ppm and it is 42.3ppm during operation. There are a significant difference showing that the P value is lower than 0.05. Assessing exposure level to nitrous oxide based on nurses' working positions, the exposure levels do not show significant difference( P>0.005). And $N_2O$ in active sampling method is higher than passive sampling method(P<0.05).

• Proceedings of the KSRS Conference
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• 2000.04a
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• pp.166-171
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• 2000

밀티빔 음향 측심기 (Multibeam Echo Sounder)는 탐사선에 수직방향으로 해저면을 주사(Swath)하여, 한번의 송수신(Ping)으로 다중의 빔자료를 얻을 수 있는 측심기로, 해저면에 반사되어 되돌아오는 음파의 음압을 기록하고, 사이드 스캔 소나 자료도 동시에 취득하는 기능을 가지고 있으므로, 측심된 해저 지형(Bathymetry)과 해저 지형을 덮고 있는 해저면의 퇴적 상황(Sediment Environment)도 동시에 얻을 수 있는 다목적 측심기이다. 본 논문에서는 L3사의 Sea Beam 2100 멀티빔 음향 측심기를 통해 얻은 자료를 처리하여, 3차원 공간 데이터인 DEM(Digital Elevation Model)을 생성하고, VRML을 이용한 웹상에서의 해저 지형 가시화를 통해, 세계 어느 곳에서나 웹을 통하여 쉽게 정보를 공유할 수 있는 3차원 해저 지리 정보 시스템의 구현을 목적으로 한다. 멀티빔 음향 측심기를 통해 얻어진 자료는 항해 자료 보정, 음속 보정, 빔 좌표 계산과 분리, 오측심 자료 제거, 조석 보정 등의 단계를 거쳐 측심자료의 정확도 및 신뢰도를 높이는 과정을 거치게 된다. 보정된 멀티빔 음향 측심자료는 무작위 점 사상(Point Topology)으로 산재 되어 있는 빔 자료를 임의의 단위영역으로 변환하는 과정을 거쳐야 하는데, 이 과정을 격자화라고 한다. 자료의 격자화를 통해 3차원 공강 데이터인 DEM 파일을 제작하고, 이 DEM 파일과 음압 영상을 이용해 웹상에서의 3차원 해저 지형의 가시화를 실현한다. 웹상에서의 3차원 지형 가시화에서 방대한 양의 지형 데이터는 데이터 전송 시간과 렌더링 시간에 치명적인 문제이다. 따라서, 렌더링 시간과 데이터 전송 시간을 단축시키기 위한, 지형 자료의 LOD(Level of Detail)를 통해, VRML을 이용한 보다 효과적인 웹상에서의 3차원 해저 지형의 가시화를 실현한다.면 기업은 고객으로 공간적인 제약으로 인한 불신을 불식시키는 신뢰감을 주게 된다. 이러한 고객서비스 향상과 물류비용 절감은 사이버 쇼핑몰이 전국 어디서나 우리의 안방에서 자연스럽게 점할 수 있는 상황을 만들 것이다.SP가 도입되어, 설계업무를 지원하기위한 기본적인 시스템 구조를 구상하게 된다. 이와 함께 IT Model을 구성하게 되는데, 객체지향적 접근 방법으로 Model을 생성하고 UML(Unified Modeling Language)을 Tool로 사용한다. 단계 4)는 Software Engineering 관점으로 접근한다. 이는 최종산물이라고 볼 수 있는 설계업무 지원 시스템을 Design하는 과정으로, 시스템에 사용될 데이터를 Design하는 과정과, 데이터를 기반으로 한 기능을 Design하는 과정으로 나눈다. 이를 통해 생성된 Model에 따라 최종적으로 Coding을 통하여 실제 시스템을 구축하게 된다.the making. program and policy decision making, The objectives of the study are to develop the methodology of modeling the socioeconomic evaluation, and build up the practical socioeconomic evaluation model of the HAN projects including scientific and technological effects. Since the HAN projects consists of 18 subprograms, it is difficult In evaluate all the subprograms simultaneously. Despite, each program is being performed under the category of HAN projects, so the common soci

• Korean Journal of Food Science and Technology
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• v.46 no.3
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• pp.276-282
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• 2014

An accurate and sensitive analytical method was established for the simultaneous determination of synephrine and n-methyltyramine contents by ultra-performance liquid chromatography (UPLC) with a fluorescence detector (FLD). A 70:30 (v/v) mixture of 10 mM sodium dodecyl sulfate (SDS) and acetonitrile was used as the mobile phase. The coefficient of correlation ($r^2$) was 0.9999 for both synephrine and n-methyltyramine, and their limits of detection (LOD) were 0.02 and 0.01 mg/kg, respectively. The percentage recoveries for synephrine and n-methyltyramine were 96.4% and 100.9%, respectively, from bitter orange (Citrus aurantium) samples. The synephrine and n-methyltyramine contents were 38.07-118.21 mg/kg and 0.27-0.56 mg/kg, respectively, in the orange fruit samples, while they were 14.61-120.39 mg/kg and up to 3.34 mg/kg, respectively, in the tested commercial orange juice samples. The differences in synephrine and n-methyltyramine content between orange fruit and commercial orange juice were not significant (p<0.05). These results suggest that UPLC-FLD can be applied to develop an analytical method of quality control for commercial orange juice.

• Korean Journal of Food Science and Technology
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• v.48 no.5
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• pp.405-412
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• 2016

Illegally adulterated compounds, such as impotency drugs and their synthetic analogues, which have been purported to enhance sexual potency or mood, have been constantly detected in foods including dietary supplements. The adulterated foods with these illegal compounds may threaten public health because their safety and efficacy have not been verified. This study was aimed at investigating illegal compounds in foods and counterfeit products. 54 illegal compounds were assayed using a simultaneous analytical method involving liquid chromatography equipped with photo diode array (LC-PDA) and LC coupled with tandem mass spectrometry (LC-MS/MS). The method was validated in terms of selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision and accuracy. In 48 of 161 samples, we identified 7 different illegal compounds, including sildenafil, tadalafil, chlropretadalafil, demethylsildenafil, dimethyl-thiosildenafil, icariin and yohimbine. When purchasing products marketed for erectile dysfunction or aphrodisiacs, ulmost care should be taken owing to the possible presence of these illegal compounds.

• Journal of Food Hygiene and Safety
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• v.27 no.4
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• pp.332-338
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• 2012

A simple and sensitive analytical method was developed using gas chromatography with electron capture detector (GC-ECD) and gas chromatography-mass spectrometry (GC-MS) for determination of Picoxystrobin in agricultural products (apple, hulled rice, mushroom, pepper, soybean, and mandarin). Picoxystrobin residues were extracted with acetonitrile, partitioned with saline water, and then they were cleaned up on a florisil solid-phase extraction (SPE) cartridge to obtain an extract suitable for analysis by GC-ECD and GC-MS. The method was validated using 6 agricultural product samples spiked with Picoxystrobin at different concentration levels (0.02, 0.05 and 0.5 mg/L). Average recoveries of Picoxystrobin (using each concentration three replicates) ranged 64.0~98.3% with relative standard deviations less than 10%, calibration solutions concentration in the range 0.1~5 mg/L, and limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.02 mg/L, respectively. The result showed that the developed analytical method is suitable for Picoxystrobin determination in agricultural products.

• Journal of Food Hygiene and Safety
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• v.29 no.4
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• pp.312-315
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• 2014

The present study demonstrated the development and validation of the method for the quantification of phenol in food using gas chromatography coupled with mass spectrometry (GC-MS). After spiking of internal standard (Phenol-$d_5$) to food, those samples were extracted with organic solvent mixture (acetone : dichloromethane = 1 : 1, v/v) using ultra sonic extractor and cleaned by gel permeation chromatography (GPC) technique. The amount of phenol was determined by GC/MS. To validate the developed method, we evaluated parameters were the selectivity, linearity, accuracy, precision, and recovery. To demonstrate the selectivity of the method, blank samples of rice, corn, and fish(mackerel) were prepared and subjected to GC-MS analysis. To verify the linearity of the method, six different standard concentrations of phenol at 0.01, 0.05, 0.1, 0.5, 1 and 2.5 mg/kg were evaluated. The correlation coefficient ($r^2$) of calibration curve was 0.9999. The recovery rate for phenol standard calculated by internal standard method were 82.2~101.5% for samples fortified with 0.25, 0.50, and 1.0 mg/kg, respectively. Also the repeatability and reproducibility for validation of precision were 0.2~5.5%. According to the result of the validation, this established method was suitable for AOAC guideline. The limit of detection (LOD) for phenol analysis were 0.03~0.1 mg/kg, and the limit of quantification (LOQ) were 0.1~0.3 mg/kg. Therefore, we established the optimal analysis method for determination of phenol in food using GPC and GC/MS.