利用氣相層析串聯質譜儀建立化粧品中禁限用成分分析方法   全文下載

Determination of Banned and Restricted Compounds in Cosmetics by GC-MS/MS

本研究利用氣相層析串聯質譜儀（GC-MS／MS）建立簡單、快速分析化粧品中呋喃香豆素類化合物等8種禁、限用化合物之方法。檢體以丙酮萃取呋喃香豆素等8種禁、限用化合物，經HP-5MS UI層析管柱分離後，利用電子游離（EI）及多重反應監測（Multiple reaction monitoring, MRM）模式進行鑑別與含量測定，其中黃樟素（Safrole）、6-甲基香豆素（6-Methylcoumarin）、8-甲氧基補骨脂（8-methoxypsoralen, 8-MOP）、5-甲氧基補骨脂（5-methoxypsoralen, 5-MOP）及三甲沙林（Trioxsalen）之線性範圍為5－100 ng／mL，另碘丙炔正丁胺甲酸酯（Iodopropynyl butylcarbamate, IPBC）、合成麝香（Musk ambrette）及歐前胡素（Impreatorin）之線性範圍為10－100 ng／mL，線性相關係數皆為0.999以上，空白檢體之平均添加回收率介於80.9－127.4％，變異係數為7.8％以下。呋喃香豆素及其他禁、限用成分之定量極限除Imperatorin、Musk ambrette及IPBC為0.2 ppm外，其餘皆可達0.1 ppm。利用本方法檢測30件市售化粧品檢體，結果均未檢出Musk ambrette、Safrole及呋喃香豆素類化合物等禁用成分；另標示含有IPBC者，共計12件，檢出之含量均符合法規限量。

A gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) method was developed to determine furanocoumarins (5-methoxypsoralen, 8-methoxypsoralen, trioxsalen, imperatorin), iodopropynyl butylcarbamate, safrole, musk ambrette and 6-methylcoumarin in cosmetics. Samples were extracted by acetone and separated on a HP-5MS UI column. The compounds detection was on multiple reaction monitoring (MRM) mode. The linearities of 8 compounds were evaluated by several concentrations of standard compounds between the range of 5-100 ng/mL individually. The coefficients of correlation (r) were all higher than 0.999. The recoveries were conducted by spiking 3 different concentration levels, and were between 80.9% and 127.4% for all compounds.The relative standard deviations (RSDs) were all below 7.7%. The limits of quantitation (LOQs) of 8 compounds ranged were from 0.1 ppm to 0.2 ppm. The surveillance results of 30 commercial cosmetic samples showed that no sample contained furanocoumarins, safrole and musk ambrette. There were 12 samples labeled IPBC in their packages, the testing results showed all were complied with the regulation.