화장품에 함유된 미량의 프탈레이트 함량을 정확히 분석하기 위한 가스크로마토그래피-질량분석 시험법 및 그 시험법의 유효성 Accurate Analysis of Trace Phthalates and Method Validation in Cosmetics using Gas Chromatography with Mass Spectrometric Detection원문보기
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 프탈레이트 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 내부표준물질로 두 물질의 중수소치환체인 DBP-$d_4$,와 DEHP-$d_4$를 사용하였다. 시험법의 유효화를 시행한 결과 본 시험법이 ppm 농도의 프탈레이트 정량분석에 적합함을 확인하였으며, 네일락카와 헤어스프레이 제품에 약 $25{\mu}g/g$의 농도로 표준물질을 첨가하여 분석한 회수율은 95 - 106.1 % 범위였고, % 상대표준편차 값은 3.9 % 이하였다.
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 프탈레이트 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 내부표준물질로 두 물질의 중수소치환체인 DBP-$d_4$,와 DEHP-$d_4$를 사용하였다. 시험법의 유효화를 시행한 결과 본 시험법이 ppm 농도의 프탈레이트 정량분석에 적합함을 확인하였으며, 네일락카와 헤어스프레이 제품에 약 $25{\mu}g/g$의 농도로 표준물질을 첨가하여 분석한 회수율은 95 - 106.1 % 범위였고, % 상대표준편차 값은 3.9 % 이하였다.
An effective, environmentally friendly analytic methods using gas chromatography with mass spectrometric detector (GC-MSD) have been developed for the quantitative analysis of trace phthalate levels in cosmetics such as nail lacquer and hair spray. Since such cosmetics are largely comprised of organ...
An effective, environmentally friendly analytic methods using gas chromatography with mass spectrometric detector (GC-MSD) have been developed for the quantitative analysis of trace phthalate levels in cosmetics such as nail lacquer and hair spray. Since such cosmetics are largely comprised of organic solvents, conventional clean-up methods that have been widely used for phthalate analyses are in adequate. In addition, analysis of trace phthalate levels is notorious for its sensitivity to contamination, which causes high analytical values. A direct sample dilution method using an organic solvent was adopted to the sample preparation process to determine the exact amounts of phthalates and simultaneously avoid the high risk of secondary contamination. The method has many advantages including high accuracy, sensitivity, and simplicity in sample preparation. Dibutyl phthalate (DBP) and di (2-ethylhexyl) phthalate (DEHP) were selected for analysis because they have been frequently detected in cosmetics and consistently reported as endocrine disruptors in humans and animals. Internal standard method using two deuterium substitutes (DBP-$d_4$, DEHP-$d_4$) as the internal standard was also used. The results of 'Method validation' showed the capabilities of this method for the routine analysis of phthalates at the ppm level. The recovery ranges were between 95 % and 106.1 %, and relative standards deviations (RSD) were less than 3.9 % in fortified nail lacquer and hair spray samples at the concentration of $25{\mu}g/g$.
An effective, environmentally friendly analytic methods using gas chromatography with mass spectrometric detector (GC-MSD) have been developed for the quantitative analysis of trace phthalate levels in cosmetics such as nail lacquer and hair spray. Since such cosmetics are largely comprised of organic solvents, conventional clean-up methods that have been widely used for phthalate analyses are in adequate. In addition, analysis of trace phthalate levels is notorious for its sensitivity to contamination, which causes high analytical values. A direct sample dilution method using an organic solvent was adopted to the sample preparation process to determine the exact amounts of phthalates and simultaneously avoid the high risk of secondary contamination. The method has many advantages including high accuracy, sensitivity, and simplicity in sample preparation. Dibutyl phthalate (DBP) and di (2-ethylhexyl) phthalate (DEHP) were selected for analysis because they have been frequently detected in cosmetics and consistently reported as endocrine disruptors in humans and animals. Internal standard method using two deuterium substitutes (DBP-$d_4$, DEHP-$d_4$) as the internal standard was also used. The results of 'Method validation' showed the capabilities of this method for the routine analysis of phthalates at the ppm level. The recovery ranges were between 95 % and 106.1 %, and relative standards deviations (RSD) were less than 3.9 % in fortified nail lacquer and hair spray samples at the concentration of $25{\mu}g/g$.
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제안 방법
Hair spray and nail lacquer samples, which were prepared in concentrations of 25.0 µg/g of each DBP and DEHP, were analyzed.
According to our experimental observations, the sample preparation meth-ds discussed above are ineffective for phthalate analysis of these cosmetics. In this study, we adopted a direct sample dilution method with an organic solvent, and quantified DBP, and DEHP at low levels in nail cosmetics and hair sprays with GC-MSD. Two phthalates (DBP and DEHP) were selected for analyses because they have been identified in these cosmetics and are possible endocrine disruptors in humans.
Further, it is highly accurate because they eliminate phthalate contamination during the analytical process and use deuterium derivatives as internal standards. Method validation showed that these methods are capable of routinely detecting DBP and DEHP in nail cosmetics and hair sprays at the ppm level analysis.
This study was an outgrowth of long-term unsuccessful attempts to test various preparation methods such as SPE, LLE, and adsorption column chromatography to establish an adequate analytical method that would enable analysis of organic solvent-based samples.
대상 데이터
The GC-MSD system used was the 6890GC (Agilent, USA), which included capillary column split/splitless EPC inlet and liquid autosampler, 5975B inert XL MSD (Agilent, USA), and Mass Chemstation data system. The analytical column was HP-5MS (30 m × 0.
데이터처리
The calibration curve was obtained using first-order and second-order least squares regression. The correlation coefficients (r2, criterion : > 0.
이론/모형
We can compensate that deviation by using internal standard. The use of internal standards was vital to the accuracy and reliability of results obtained with our GC-MSD method.
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