化粧品禁用重金屬檢驗方法探討   全文下載

Development of the Method for Prohibited Heavy Metals in Cosmetics

化粧品重金屬殘留是民眾非常關心的議題，雖然重金屬無化粧品常見之宣稱用途，卻可能隨色素或其他成分及製程微量殘留於最終製品中，因此衍生安全疑慮。目前化粧品禁止使用或內含於禁止使用成分（如鈷（Co）和鎳（Ni））之重金屬元素達12種，其中砷（As）、鎘（Cd）、汞（Hg）、鉛（Pb）訂有殘留限量。本研究透過感應耦合電漿質譜儀（ICP-MS），以微波輔助酸消化法（Microwave assisted acid digestion），完成建立分析12種重金屬元素之方法。本法以濃硝酸12 mL及30%過氧化氫3 mL進行檢體消化，除分析硒（Se）時於定容至50 mL前，另加入異丙醇0.25 mL外，其餘均直接定容至50 mL，以濾膜過濾後進行分析。本研究分析之重金屬元素，除硒（Se）之線性範圍為10-200 ng/mL及鋯（Zr）為1-10 ng/mL外，其餘均為0.5-10 ng/mL，並依個別元素之測定質量數，自鍺（Ge）、銠（Rh）或鉍（Bi）選擇適當者作為內部標準品，最終濃度均為5 ng/mL（分析硒（Se）時採用銠（Rh）20 ng/mL），相關係數（r）均在0.999以上。添加回收試驗選用洗髮精、乳液類及唇膏做為測試檢體，進行添加回收試驗，其回收率均介於83.2-118.7%間。各元素之定量極限除鋯（Zr）為0.2 ppm、硒（Se）為2.0 ppm外，其餘元素均為0.1 ppm。

Heavy metal residues in cosmetics is an issue which catches public concern. Although most of residual heavy metals do not have direct functions or effects in cosmetics, they may present in the final products along with pigments or other ingredients during manufacturing process, and therefore cause safety concerns. At present, there are 12 heavy metals prohibited in cosmetics, among them maximum residue limits are set on arsenic, cadmium, mercury and lead. In this study, an analytical method for the determination of 12 heavy metals was developed by utilizing microwave digestion and ICP-MS. Samples were digested with a mixture of 12 mL concentrated HNO_3 and 3 mL H_2O_2 (30%) using a microwave digestion system. The digested samples were transferred and volume to 50 mL with deionized water. Additional isopropanol (0.25 mL) was required to add in selenium test samples prior to volume. The linearities of zirconium was obtained at 1-10 ng/mL, selenium was 10-200 ng/mL, and others were 0.5-10 ng/mL. Germanium (Ge), rhodium (Rh) and bismuth (Bi) were used as internal standards in correspondence to target heavy metals. The coefficients of correlation (r) obtained were all higher than 0.999. For recovery studies, heavy metals were spiked to shampoo, cream and lipstick. The average recoveries were 81.5% to 118.7% in shampoo, 84.5% to 111.9% in creams and 83.2% to 114.9% in lipsticks. The limit of quantification (LOQ) of all elements were 0.1 ppm, except 0.2 ppm for zirconium and 2.0 ppm for selenium.