본 연구는 조제유류 중 지방산에 대해 최신 분석법을 마련하고자 수행하였다. 조제유류 중 지방산 함량 분석을 위해 GC를 이용한 분석법을 확립하고 시중에 유통 중인 제품을 대상으로 적용성을 검토하였다. 분석법 검증은 특이성, 직선성, 검출한계 및 정량한계, 정확성, 정밀성에 대해 수행되었다. Linoleic acid 및 α-linolenic acid의 0.1-5 mg/ mL 농도범위에서 R2=0.999 이상의 우수한 직선성을 확인할 수 있었다. Linoleic acid 및 α-linolenic acid의 LOD는 각각 0.06 mg/mL, 0.01 mg/mL, LOQ는 각각 0.16 mg/mL, 0.03 mg/mL였다. 표준인증물질 분석을 통해 정확성을 검토 하였으며, linoleic acid 및 α-linolenic acid의 회수율은 각각 100.8%와 101.1%로 확인하였다. 정밀성을 검토한 결과 시료 채취량에 따른 반복성은 linoleic acid 1.4-2.9%, α- linolenic acid 1.1-2.7%이었고, 실험실간 재현성은 각각 2.8%, 1.5%임을 확인하였다. 본 연구에서 확립된 분석법을 적용하여 국내 유통 중인 조제유류 및 조제식 제품 12건에 대해 적용성 검토를 실시한 결과 전체 시료에서 분석이 용이 하였으며, 모두 기준·규격에 적합함을 확인하였다. 본 결과로부터 확립된 GC를 이용한 분석법은 조제유류 중 지방산 함량을 확인하기에 적합함을 확인하였으며 국내 식품 영양 성분의 관리 기반을 강화하는데 기여할 것으로 사료된다.
According to the development of GC equipment, it has been possible to analyze the low level of ambient VOCs concentration. In this study, the limit of detection and the limit of quantitation were estimated for two GC equipments of the VOCs analysis, which would contribute to improve the quality of VOCs analysis results. The results of %RSD for ten standard solutes showed a great reproducibility in terms of detection time and detection area. The limit of detection and the limit of quantitation in SRI GC appeared to be 0.175 ppb and 0.583 ppb for benzene, and 0.223 ppb and 0.743 ppb for toluene, respectively. On the other hand, The limit of detection and the limit of quantitation in FISON GC appeared to be 0.149 ppb and 0.496 ppb for benzene, and 0.094 ppb and 0.313 ppb for toluene, respectively.
We studied an analytical method for 4 organic acids will be regulated in 2010 using on-line thermal desorber with gas chromatograph/flame ionization detector. Results for each compounds showed good linearity(r² > 0.99) and good precision(RSD < 3%). Minimum detection limit values are about 2~3ppb when we sampled 1.5 L. These values will be reduced to 0.4~0.5 ppb when sampling 10L. We analyzed the 56 ozone precursor standard gas using the same method to see if there are any peaks to be overlapped in ambient air and the results showed that there is no peak overlapped. The linearity, precision and MDL in this study satisfied the guideline of Korean standard method for 4 organic acids. This analytical method in this study could be utilized effectively as on-line monitoring instrument to detect 4 organic acids.
In this study, the most effective salting-out effect has been examined in terms of application of various inorganic salts (NaCl, Na₂S0₄, NaHSO₃) using Alkali impregnated filter-Headspace-GC/FID. Five various VFAs (propionic acid (99.5%), r-butyric acid (99%), butyric acid (99%), i-valerie acid (99%), valerie acid (99%)) have been used. VFAs have been analyzed by adding 30%, 70%, 100%, 150%, 200% of different inorganic salts with HS-GC/FID. The efficiency of salting-out effect was obtained from the values of peak area in chromatogram. The most effective salting-out effect for applired inorganic salts was observed at 100% saturation. It was confirmed NaHSO₃ for salting-out effect was the best among inorganic salts. In addition, NaHSO₃ showed more efficiency of salting-out effect than NaCl as molecular weight of VFAs increases.
In this study, we attempt to analyze for 4 compounds (MEK, MIBK, n-Butyl acetate, i-Butyl alcohol) in ambient air using on-line thermal desorber (on-line TD) with gas chromatograph/flame ionization detector (GC/FID). These compounds will be regulated by KMOE (Korean ministry of environment) within 2010. We tested two different experimentation. First, we try to find the influence of Nafion dryer for the 4 compounds. Second, we want to know basic analytical characteristic of target compounds through the linearity, reproducibility, and minimum detection limit. According to this study, target compounds are removed in Nafion dryer more than 80 percent, respectively. So, we progressed next experimentation progressed without Nafion dryer using hydrophobic cold trap. Results for each compounds showed good linearity (r²=0.99 upper) and good precision (RSD=1 % below). In additional, we analyzed the ozone precusors standard gas (56 compounds) using the same method to see if there are any peaks to be overlapped in ambient air. These results showed that there is no peak overlapped. This means that analytical system of this study could be used on-line analytical system. Minimum detection limit (MDL) value for this system are less than minimum malodor threshold concentration.
Volatile fatty acids (VFAs) are malodor compounds which are produced from the decomposition of animal or plant species. It is very difficult to detect VFAs due to their strong adsorptive properties. In this study we develop an analytical method using headspace-GC/FID with an alkali-impregnated filter sampling. The addition of NaCl and H₂S0₄ makes the salt-out and pH-lowering effect, respectively. The high boiling points (141~185℃) and vapor pressures require a high temperature and long heating time for the standard sample in vials to reach an equilibrium. The analytical response was highest when the absolute quantity in the sample was 5 mL in a 22 mL vial. The addition of NaCl for the salt-out effect can give a higher sensitiviry by a factor of 1.1~4.2 than that of Na₂SO₄. The mass amount of 4.6 g of NaCl can result in a higher sensitivity, which is higher than the supersaturated solubility of 4.2 g. The concentration of H₂SO₄ is as low as 2% (v/v). When the concentration range is 8.3 -562.1 ppb, a coefficient of R²~0.99 can be obtained for the five VFAs samples. The analytical errors in a reproducibility test are less than 10% and the detection limit is estimated to be 0.05~0.1 ppb. Our headspace-GC/FID analytical method can be utilized to effectively detect the five kinds of VFAs which shall be restricted in Republic of Korea from the year of 2010.
An analytical method for trimethylamine in ambient air was developed, using headspace gas chromatography with flame ionization detection. Trimethylamine was collected on the acid filter which was impregnated sulfuric aicd in the 47 ㎜ diameter of glass fiber filter. Trimethylamine collected on the acid filter was regenerated in the headspace vial and introduced into the GC analytical column directly. Several parameters such as sample volume, equilibrium temperature and time, and slurry method of filter were optimized to provide maximum detection response. Resolution power also compared according to liquid phase of analytical column. The detection limit of method was 0.13 ppb with 50 L sampling volume. The developed acid filter method is easy to deal with the field sampling and the method was adopted as the standard method for odor analysis in Korea.
This study assessed the analysis method for measuring volatile organic silicon compounds (namely as siloxanes) by usinggas chromatography with flame ionization detector. Calibration standard gas was made in a laboratory by using six volatileorganic silicons as model gas. Two different types of working gas were prepared to evaluate quality control in GC-FIDanalysis. Less than 0.2 RSD% of repeatability of retention time was observed in the analysis of calibration standard gas. Inthe linearity test, the highest coefficient of determination (R2) was found to be 0.997 for L2 among volatile organic siliconcompounds. This study demonstrated that quantification of volatile organic silicon compounds can be performed by usingGC-FID analysis with direct injection mode, and the GC calibration can be covered by the gas-phase standard method.
A new method based on solid phase microextraction(SPME), coupled with GC/FID, has been developed for the determination of PCE and TCE in water samples. The experimental parameters affecting the SPME process (i.e, kinds of fibers, extraction time, desorption time, extraction temperature, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. The coefficients of determination (R2) for PCE and TCE were 0.9951 and 0.9831, respectively when analytes concentration ranges from 10 to 300㎍/L. The relative standard deviations were 3.4 and 2.1% for concentration of 10㎍/L(n=5), respectively. The detection limits of PCE and TCE were 0.5 and 1.3㎍/L, respectively.