• Analytical Science and Technology
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• v.20 no.2
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• pp.115-123
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• 2007

The heterocyclic amines (HAs) are a family of mutagenic/carcinogenic chemicals formed from the cooking of muscle meats such as beef, meat, fowl, and fish. A major draw back in the analysis of HAs from foods is their very low level of concentration (ng/g) and a number of matrix interferences in samples. Solid-phase extraction (SPE) is one of the procedures widely used for the extraction and purification of HAs in food samples. In this study, several SPE procedures of HAs determination were performed. Recoveries of the HAs were obtained from comparing a matrix such as a standard methanolic solution and pre-cooked meat extracts. Recovery values were ranging between 25.3 and 93.0 % at a concentration of 25.0 ng/g. HAs were determined with high sensitivity by micro-HPLC (${\mu}$-HPLC) analysis with electrospray ionization mass spectrometry (ESI-MS). Another developed method, which is freezing filtration method, shows better extraction recoveries and good precisions. The established method will be applicable to monitoring of heterocyclic amines from the cooked meat.

• The Korean Journal of Nuclear Medicine Technology
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• v.22 no.2
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• pp.74-78
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• 2018

Purpose $[^{11}C]$acetate has been proved useful in detecting the myocardial oxygen metabolism and various malignancies including prostate cancer, hepatocellular carcinoma, renal cell carcinoma and brain tumors. The purpose of study was to improve the radiosynthesis yield of $[^{11}C]$acetate on a automated radiosynthesis module. Materials and Methods $[^{11}C]$acetate was prepared by carboxylation of grignard reagent, methylmagnesium chloride, with $[^{11}C]$$CO_2$ gas, followed by hydrolysis with 1 mM acetic acid and purification using solid phase extraction cartridges. The effect of the reaction temperature ($0^{\circ}C$, $10^{\circ}C$, $-55^{\circ}C$) and cyclotron beam time (10 min, 15 min, 20 min, 25 min) on the radiosynthesis yield were investigated in the $[^{11}C]$acetate labeling reaction. Results The maximum radiosynthesis yield was obtained at $-10^{\circ}C$ of reaction temperature. The radioactivities of $[^{11}C]$acetate acquired at $-10^{\circ}C$ reaction temperature was 2.4 times higher than those of $[^{11}C]$acetate acquired at $-55^{\circ}C$. Radiosynthesis yield of $[^{11}C]$acetate increased with increasing cyclotron beam time. Conclusion This study shows that radiosynthesis yield of $[^{11}C]$acetate highly dependent on reaction temperature. The best radiosynthesis yield was obtained in reaction of grignard reagent with $[^{11}C]$$CO_2$ at $-10^{\circ}C$. This radiolabeling conditions will be ideal for routine clinical application.

• The Korean Journal of Pesticide Science
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• v.11 no.2
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• pp.87-94
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• 2007

Pyrethroid insecticide have widely been used for agricultural sector and residential environments. To assess the exposure of insecticide which is absorbed through skin the analysis of urinary metabolite is essential. At present, the urinary 3-PBA was analyzed using liquid-phase extraction. But LPE have many limitations, such as long pre-treatment time and low recovery. So, this study was conducted to determine the optimum conditions for analysing 3-PBA in urine using solid phase extraction. Furthermore, this study intend to investigate the relation of concentrations of pyrethroid, deltamethrin in air and 3-PBA in urine. The optimum condition for hydrolysis was found to be done with hydrochloric acid for one hour. The recovery rates of 3-PBA were $84.6%{\pm}1.2%$, $54.8{\pm}0.9%$, $99.8{\pm}1.2%$ with XAD-2, XAD-7, XAD-16 using as the aborbents and acetone as eluents respectively. But acetonitrle and methanol gave low recovery rate and methyl cellosolve could not elute the compound. The amount of acetone for elution were 6mL, 9mL, 3mL for XAD-2, XAD-7, XAD-16 as absorbents respectively. The non-absorbed rates was $0.8{\pm}0.5%$, and $0.7{\pm}0.3%$ under XAD-16, mesh size 140-200, amount of resin 1.4g and the flow rate of eluent was 0.1mL/min. In the concentration process, we obtained 11 times higher concentration of material. The amounts of urinary 3-PBA were. The LODs of 3-PBA and deltamethrin were 0.004 mg/L, 0.038 mg/L, respectively. The further research of minute monitoring which include spray pattern, environmental condition is needed And more research about the relation between total pyrethroid exposure and urinary various metabolite are also necessary.

• Korean Journal of Pharmacognosy
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• v.43 no.3
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• pp.250-256
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• 2012

In order to extract the curcuminoid such as curcumin, demethoxycurcumin (DMC), and bisdemethoxycurcumin (BDMC) in turmeric (Curcuma longa), solvent extraction methods (dipping and ultrasonic extraction method) and solid-phase extraction (SPE) were used. RP-HPLC (reverse-phase high-performance liquid chromatography) and TLC (thin-layer chromatography) were used for identification and analysis the three curcuminoid. From the experimental results, it is evident that the percentage of curcuminoid extracted from turmeric by ultrasonic extraction method was higher than dipping method. The percentage of curcumin extracted from turmeric by pure methanol was higher than any aqueous methanolic composition. Moreover, the total peak area of three curcuminoid was above 92% in RP-HPLC using solid-phase extraction. These results will form a database for investigating the constituents of natural products and the resources of pharmaceutical, nutrition, and cosmetic products.

• Journal of Korean Society of Environmental Engineers
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• v.31 no.9
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• pp.825-830
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• 2009

Pharmaceutical compounds enter the water environment through the diverse pathways. Because their concentration in the water environment was frequently detected in the level of ppt to ppb, the monitoring system should be optimized as much as possible for finding appropriate management policies and technical solutions. One Factor At a Time (OFAT) approach approximating the response with a single variable has been preferred for the optimization of LC-MS/MS operational conditions. However, it is common that variables in analytical instruments are interdependent. Therefore, the best condition could be found by using the statistical optimization method changing multiple variables at a time. In this research, response surface analysis (RSA) was applied to the LC-MS/MS analysis of emerging antibiotic compound, sulfamethoxazole, for the best sensitivity. In the screening test, fragmentation energy and collision voltage were selected as independent variables. They were changed simultaneously for the statistical optimization and a polynomial equation was fit to the data set. The correlation coefficient, $R^2$ valuerepresented 0.9947 and the error between the predicted and observed value showed only 3.41% at the random condition, fragmentation energy of 60 and collision voltage of 17 eV. Therefore, it was concluded that the model derived by RSA successfully predict the response. The optimal conditions identified by the model were fragmentation energy of 116.6 and collision voltage of 10.9 eV. This RSA can be extensively utilized for optimizing conditions of solid-phase extraction and liquid chromatography.

• Korean Journal of Food Science and Technology
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• v.30 no.3
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• pp.638-643
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• 1998

The volatile flavor components in Takju made from mashed glutinous rice and barley rice were identified by GC and GC-MS using polar column. Twenty eight kinds of flavor compounds including 10 alcohols, 9 esters, 2 acids, 7 aldehydes were identified. At the beginning of fermentation 14 kinds of volatile components were detected and the kinds of volatile components were increased up to maximum after fermentation for 16 days. The contents of volatile components in the sample made from glutinous rice contained slightly higher than the sample made from barley rice. Ethyl alcohol, n-propyl alcohol, iso-amyl alcohol, n-hexyl alcohol, hexenyl alcohol, 2-phenylethyl alcohol, ethyl acetate, ethyl succinate, 2-phenylethyl acetate, butyic acid, benzaldehyde and 3-methoxybenzaldehyde were detected in the both of the sample throughout the fermentation process. Five kinds of aldehyde including ethyl propionate, iso-amyl acetate, ethyl caprylate and ethylphenyl acetate were detected only in the sample fermented for 16 days. The main components of the both sample were ethyl alcohol, iso-amyl alcohol, 2-phenylethyl alcohol, 2-phenylethyl acetate, hexenyl alcohol and iso-butyl alcohol. Besides ethyl acetate and benzaldehyde from glutinous rice Takju and hexenyl alcohol from barley rice Takju were found as main components.

• Journal of the Korean Society for Marine Environment & Energy
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• v.17 no.1
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• pp.27-35
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• 2014

The headspace solid-phase microextraction (HS-SPME) followed by gas chromatography/mass spectrometry procedure has been developed for the simultaneous determination of petroleum aromatic hydrocarbons such as benzene, toluene, ethylbenzene and xylene isomers (BTEX) and polycyclic aromatic hydrocarbons (PAHs) in seawater. The advantages of SPME compared to traditional methods of sample preparation are ease of operation, reuse of fiber, portable system, minimal contamination and loss of the sample during transport and storage. SPME fiber, extraction time, temperature, stirring speed, and GC desorption time were key extraction parameters considered in this study. Among three kinds of SPME fibers, i.e., PDMS ($100{\mu}m$), CAR/PDMS ($75{\mu}m$), and PDMS/DVB ($65{\mu}m$), a $65{\mu}m$ PDMS/DVB fiber showed the most optimal extraction efficiencies covering molecular weight ranging from 78 to 202. Other extraction parameters were set up using $65{\mu}m$ PDMS/DVB. The final optimized extraction conditions were extraction time (60 min), extraction temperature (50), stirring speed (750 rpm) and GC desorption time (3 min). When applied to artificially contaminated seawater like water accommodated fraction, our optimized HS-SPME-GC/MS showed comparable performances with other conventional method. The proposed protocol can be an attractive alternative to analysis of BTEX and PAHs in seawater.

• Journal of the Korean GEO-environmental Society
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• v.11 no.5
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• pp.61-67
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• 2010

In this study, Solid-phase microextraction (SPME) with GC/FID was studied as a possible alternative to liquid-liquid extraction for the analysis of chlorinated solvents (PCE and TCE) and these by-products (cis-DCE, VC, and Ethylene). Experimental parameters affecting the SPME process (such as kind of fibers, adsorption time, desorption time, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. Experimental parameters such as CAR/PDMS, adsorption time of 20 min, desorption time of 5 min at $250^{\circ}C$, headspace volume of 50mL, sodium chloride (NaCl) concentration of 25% combined with magnetic stirring were selected in optimal experimental conditions for analysis of chlorinated solvents and these by-products. The general affinity of analytes to CAR/PDMS fiber was high in the order PCE>TCE>cis-DCE>VC>Ethylene. The linearity of $R^2$ for chlorinated solvents and these by-products was from 0.912 to 0.999 when analyte concentrations range from $10{\mu}g/L$ to $500{\mu}g/L$, respectively. The relative standard deviation (% RSD) were from 2.1% to 3.6% for concentration of $500{\mu}g/L$ (n=5), respectively. Finally, the limited of detection (LOD) observed in our study for chlorinated solvents and these by-products were from $0.5{\mu}g/L$ to $10{\mu}g/L$, respectively.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.20 no.2
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• pp.111-118
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• 2010

연구목적: 본 연구는 일반인의 비직업적 노출에 대한 혈중 16종의 다환방향족탄화수소(PAHs) 의 농도르 분석하여 PAHs의 백그라운드 노출 농도를 평가하는 것이다. 내용 및 방법: 농촌지역에 거주(비직업적 노출로서 16종 다환방향족탄화수소가 특정한 환경오염을 받지 않은 지역에 거주)하는 156명의 연구 참여자의 혈중 16가지 다환방향족탄화수소 농도의 기하평균치를 간접흡연군, 구운 음식물섭취군과 각대조군을 비교 하였다. 혈중 16종의 다환방향족탄화수소의 농도는 질량분석기를 장착한 가스크로마토그라피법과 헤드스페이스 마이크로고체상 추출법에 의하여 분석하였다. 결과: 연구참여자 중, 간접흡연자들에서 4종의 다환방향족탄화수소 아세나프틸렌(p<0.01), 아세나프텐(p<0.1), 플로렌(p<0.01), 피렌(p=0.05)가 대조군 보다 유의하게 높았다. 또한 구운육류와 생선 섭취군에서는 벤조(a)피렌(p<0.1)이 대조군 보다 유의하게 높았다. 결론: 간접흡연과 구운음식물 섭취는 비직업적 노출에서 다환방향족탄화수소 노출원의 가능성이 높다고 추정된다. 혈중 다환방향족탄화수소는 한국일반인의 비직업적 노출 농도로 사용 가능하다고 생각된다.

• Journal of Korean Society on Water Environment
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• v.26 no.4
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• pp.622-628
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• 2010

In this study, Solid-phase microextraction (SPME) with GC/FID was studied as a possible alternative to liquid-liquid extraction for the analysis of BTEX and MTBE. Experimental parameters affecting the SPME process (such as kind of fibers, adsorption time, desorption time, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. Experimental parameters such as CAR/PDMS, adsorption time of 20 min, desorption time of 5 min at $250^{\circ}C$, headspace volume of 50 mL, sodium chloride (NaCl) concentration of 25% combined with magnetic stirring were selected in optimal experimental conditions for analysis of BTEX and MTBE. The general affinity of analytes to CAR/PDMS fiber was high in the order p-Xylene>Toluene>Ethylbenzene>MTBE>Benzene. The linearity of $R^2$ for BTEX and MTBE was from 0.970 to 0.999 when analyte concentration ranges from $30{\mu}g/L$ to $500{\mu}g/L$, respectively. The relative standard deviation (% RSD) were from 2.5% to 3.2% for concentration of $100{\mu}g/L$ (n=5), respectively. Finally, the limited of detection (LOD) observed in our study for BTEX and MTBE were from $7.5{\mu}g/L$ to $15{\mu}g/L$, respectively.