화장품에 사용되는 방부제로는 가격이 저렴하고 방부효과가 좋은 파라벤류, 페녹시에탄올 및 클로로페네신 등이 일반적으로 사용된다. 하지만, 최근들어 이들 방부제가 독성과 피부 자극을 유발할 수 있다는 소비자들의 인식으로 인하여 항균 작용이 있는 직쇄상 1,2-알칸디올로 대체되고 있는 추세이다. 하지만, 항균 작용의직쇄상 1,2-알칸디올도 피부에 자극을 줄 수 있어 제한적으로 사용되어야 하므로 화장품 내 함량을 관리하는것이 중요하다. 본 실험에서는 가스크로마토그래피 불꽃이온화검출기(GC/FID)를 이용하여 화장품에서 3종의직쇄상 1,2-알칸디올류 중, 1,2-pentanediol, 1,2-hexanediol, 1,2-octanediol을 동시 분석하였다. 분석법Validation 결과 특이성을 확인할 수 있었고, 3종의 직쇄상 1,2-pentanediol, 1,2-hexanediol, 1,2-octanediol의검량선은 100~1,200 μg/g의 농도 범위에서 상관계수가 0.999 이상의 양호한 직선성을 나타내었다.검출한계(LOD)와 정량한계(LOQ)는 각각 31, 40, 19 μg/g와 98, 108, 57 μg/g로 나타났다. 화장품 내 함량에 대한 정밀성(반복성)은 2.0% 이하의 상대표준편차(% RSD)를 나타냈고, 정확성(회수율)은 99.3 ~103.3%, 99.4 ~ 106.7%, 97.5 ~ 107.3%로 각각 나타났다. 따라서 화장품 내에서 3종의 1,2-알칸디올류의동시 분석이 가능함을 알 수 있었다. 본 시험법은 3종의 1,2-알칸디올류를 화장품에서 정확하게 정량하는데활용될 수 있을 것이다.
네일락카와 헤어스프레이 같은 화장품에 존재하는 미량의 프탈레이트를 정량분석하기 위하여, 가스크로마토그래피와 질량분석기를 사용한 효과적이면서 환경친화적인 분석방법을 개발하였다. 이들 화장품들은 다량의 유기용매를 함유되어 프탈레이트를 분석하기 위하여 널리 사용되는 시료의 클린업 방법이 적합하지 않았다. 더군다나 미량의 프탈 레이트 분석시에는 실험과정 중에서의 오염으로 인해 실제보다 높은 분석값을 산출하게 되는 경우가 매우 많다. 이에 정확한 함량분석 및 이차오염을 방지하기 위해 유기용매를 사용하여 시료를 직접 희석하는 시료 전처리를 적용하였다.이 분석방법은 높은 정확성, 분석감도, 그리고 시료전처리를 간략히 할 수 있는 이점을 가진다. 화장품에서의 검출되는 빈도가 높고, 사람과 동물에 영향을 미치는 환경호르몬으로 보고되는 dibutyl phthalate (DBP)와 di (2-ethylhexyl) phthalate (DEHP) 두 종의 프탈레이트를 분석대상으로 선정하였다. 정량시 그 정확도 향상을 위해서 내부표준물질로두 물질의 중수소치환체인 DBP-d4,와 DEHP-d4를 사용하였다. 시험법의 유효화를 시행한 결과 본 시험법이 ppm 농도의 프탈레이트 정량분석에 적합함을 확인하였으며, 네일락카와 헤어스프레이 제품에 약 25 μg/g의 농도로 표준물질을 첨가하여 분석한 회수율은 95 ∼ 106.1 % 범위였고, % 상대표준편차 값은 3.9 % 이하였다.
The simultaneous determination of residual pesticides was developed using a gas chromatography. In this study, a simple and reliable methodology was improved to detect 175 kinds of residual pesticides by a liquid-liquid extraction procedure, followed by chromatographic analysis by gas chromatography. The 175 kinds of residual pesticides was classified into 4 groups according to the chemical structure, column type, resolution and sensitivity. The soybean sample selected for recovery experiment was not detected any pesticides. The recovery rates were ranged from 70.6% to 119.7% in most pesticides. The relative standard deviation (RSD 0.3~5.6%) was lower than 5.6% in all cases. The limits of detection (LOD) was lower than the maximum residue levels established by Korean legislations. The method has been successfully applied to the analysis of approximately 130 real samples.
화장품 중 불순물로서 미량의 중금속이 함유되어 있는 경우 이들의 피부흡착이 알러지를 일으킬 수가 있다. 이에 중금속으로부터 안전한 화장품인지를 신속하고 정확하게 판단하는 것이 중요하여 색소원료와 화장품 중 미량의 중금속들(Pb²+, Fe²+, Cu²+, Ni²+, Zn²+, Co²+, Cd²+ 및 Mn²+)을 동시에 분석할 수 있는 이온크로마토그래피 분석법을 개발하였다. 8종의 중금속들은 이온교환 컬럼(IonPac CS5A)으로 잘 분리되었고, post-column 장치와 UV 분광기로 검출하였다. 0.1 ~ 1000 g/mL 농도범위에서 8종의 중금속들의 검량선은 선형적이었고(r² > 0.999), 검출한계는 제품이 안전한지를 판단할 수 있는 g/L 수준이었다. 피크들의 머무름 시간과 면적의 상대표준편차는 0.21 %과 0.24 %이고, 회수율은 97 ~ 104 %이다. 이 결과들은 개발된 분석방법이 화장품 중의 미량의 중금속들을 신속하고 정확하게 분석할 수 있다는 것을 보여준다. 본 분석방법은 22개 화장품과 11개 색소원료 중의 중금속들의 함량을 분석하는데 활용하였다.
The polycyclic aromatic hydrocarbons(PAHs) content in sewage sludge was determined by gas chromatography linked to ion trap mass spectrometry(GC/ITMS) with five deuterated PAHs as internal standards. The minimum detection limit was from 1.66 to 7.14 pg for individual PAH by GC/ITMS. For determining total PAHs(∑PAH) in sewage sludge 84 samples from 74 waste water treatment plants in whole country were analyzed. The average content of ∑PAH for whole samples was 3,289±3,098 μg/kg, and ranged from 142 to maximum 20,102 μg/kg. According to the number of population of the city, the areas were classified as five regions, ie. big, large, middle, small, and rural area in which the waste water treated plants were grown. The contents of PAHs were 4,689±5,503, 5,839±6,401, 3,725±2,053, 2,237±2,069, and 2,475±1,489 μg/kg, in big, large, middle, small, and rural area, respectively.
A method for the simultaneous analysis of 31 residual organic chloride pesticides was studied using gas chromatography. Prepared analytical samples were injected to gas chromatography (HP 5890 Series II plus) on the Ultra-2 column with ECD. The packing materials for column were changed as the following reagents ; florisil and alumina N. The residual solution was loaded to column and was eluted with elution solvents ; ether : benzene (2 : 8) solution, hexane : benzene (1:1) solution, dichloromethane, acetone, and methanol.
The analytical results showed that 6 kinds of organic chlorides were not detected when florisil (first condition) was used as the column packing material. The nondetected 6 kinds of organic chlorides in the first analytical condition were detected and the recoveries of thrin-pesticides were increased, in particular, captan and captafol, but the recoveries of benzene hexachloride compounds were decreased when dichloromethane and methanol were added as elution solvents (packing material was florisil as in the first condition). The recoveries of dichlorfluanid, chlorofenvinfos, folpet, and dicofol were increased and that of aldrin was increased, but those of captan and captafol were not good when alumina N was used as the packing material.
To detect simultaneously thrin-pesticides, captan, and captafol, florisil and alumina N were used as the packing materials. The elution result showed that captan and captafol were not detected. This was because the column was activated insufficiently. The analytical method was the best (31 kinds of organic chlorides in the residual pesticides were detected sharply and showed high sensitivity) when the column (packing materials were florisil and alumina N, together) was fully activated and the impurities were removed using various elution solvents.
The toxic substances (endotoxins) from the bacterial cell walls were extracted by using incubator, centrifuge, UV-Vis spectrophotometer, and their fatty acid compositions were analyze by Gas Chromatography. The lethal toxicities and pyrogenic activities of toxic substances were tested and the results were compared each other.
The results of fatty acid analyses showed that the major fatty acid of the toxic substance was tetradecanoic acid for Vibrio vulnificus, dodecanoic acid for Escherichia coli and decanoic acid for Salmonella typhimurium. These three fatty acids were the main fatty acids for three toxic substances (more than 70%). The unique points in the fatty acid compositions were that tetradecanoic acid was composed as important one (37.15%) for V. vulnificus and that the amount of hexadecanoic acid was very small (below 2%) for three toxic substances. The lethal toxicity in ICR mice of toxic substance from V. vulnificus (LD_50 was 52.5 ㎎/㎏) was similar to that of E. coli (56.5 ㎎/㎏), but weaker than that of S. typhimurium (37.5 ㎎/㎏). Toxic substance from V. vulnificus was more pyrogenic in rabbit than that from E. coli, but less than that from S. typhimurium.
Volatile organic compounds in the ambient air were gathered irregularly by normal temperature concentrating method at Odea-ri and Oceon-ri Ulsan-gun in the neighbourhood of Ulsan Petrochemical Industrial Complex and analyzed with gas chromatograph. Several hydrocarbons in common atmospheric air or emitted fugitively from the chemical plants were identified and quantified by comparison with the retention times of standard compounds. The results from several field surveys in 1992 show that the concentrations of styrene at residential area of Odea-ri and Ocheon--ri were less than 0.4 ppm, but once a while greater within the chemical plants area. When it smelled unpleasantly in these area, the concentration of hydrocarbons were also high. It was concluded that the close and long-term investigation about other odorous components but hydrocarbons will be necessary to ascertain the cause of unpleasant odor of these area.