化粧品中禁用農藥檢驗方法之建立   全文下載

Development of the Method for Banned Pesticides in Cosmetics

近年隨著健康意識抬頭，宣稱含天然或有機植物萃取成分化粧品容易吸引消費者青睞，因此許多源自植物不同部位之萃取物（如花、葉或種子等）被添加於化粧品中。然而植物於種植過程中，可能噴灑農藥或被種植於有農藥殘留的土壤中，因此化粧品可能有殘留農藥之風險，且我國化粧品禁止使用成分表已列載多項農藥為禁止使用成分。本研究以氣相層析串聯質譜儀（GC-MS/MS）建立化粧品中19項禁用農藥檢驗方法，先進行層析條件及質譜參數建置及優化，並優先選擇含植物萃取成分較高之按摩精油及乳液，以探討方法之適用性。本研究層析管柱選用DB-5MS UI，搭配電子游離（EI）及多重反應監測模式（Multiple Reaction Monitoring, MRM）偵測，於15分鐘內可完成分析，按摩精油及乳液分別經C18粉劑及Captiva EMR-Lipid固相萃取匣淨化，均可有效去除基質干擾，本研究所涉19項農藥均屬化粧品禁用成分，因此以探討分析物之偵測極限（Limit of Detection, LOD）作為方法確效，以感度最佳之離子對S/N ratio大於10、感度次佳之離子對S/N ratio大於3及波峰清晰之最低濃度為本方法之偵測極限，結果顯示19項禁用農藥於按摩精油及乳液之偵測極限介於0.01-1.0μg/g之間，並以市售宣稱含植物萃取物之按摩精油及乳液各10件測試方法適用性，結果皆未檢出。

In recent years, many extracts derived from various parts of plants, such as flowers, leaves or seeds, etc., are added to cosmetics to attract consumers’attention with the rising health awareness. However, plants may be sprayed with pesticides during their growth or even be planted in soil with pesticides residues. Therefore, trace amount of pesticides may remain in cosmetics.“The list of ingredients prohibited in cosmetic products”includes multiple pesticides. A gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) method was developed to determine 19 prohibited pesticides in cosmetics. At first, the instrument conditions for analytes were established and optimized and essential oils for massage and lotions, considered containing high plant extracts, were used to assess theapplicability of the method. In this study, DB-5MS UI column was adapted and combined with multiple reaction monitoring (MRM) for analytes detection in 15 minutes. The essential oils for massage and lotions were extracted with C18-EC and Captiva EMR-Lipid, respectively. The results showed that the purification procedure could effectively remove matrix interference. The LODs (limit of detection) of the analytes were determined at the concentration with which the S/N ratio of the precursor ion and the product ion were greater than 10 and 3, respectively, and all the peaks must be clear. The LODs of 19 analytes ranged from 0.01-1.0μg/g. The method was applied to test 10 essential oils for massage and another 10 lotions. The results showed that none of the samples contained any of 19 prohibited pesticides.