合金材質食品器具中鉛與銻之檢驗方法開發   全文下載

Development of an Analytical Method for Lead and Antimony in Metal Alloy Food Utensils and Containers

為配合衛生福利部112年1月11日公告修正之「食品器具容器包裝衛生標準」將原金屬罐之衛生標準拆分為「金屬合金類-與食品直接接觸面為金屬合金者」及「金屬合金類-與食品直接接觸面為合成樹脂塗漆者」2類，並於「金屬合金類-與食品直接接觸面為金屬合金者」之材質試驗增列鉛及銻之衛生標準分別為0.1%以下及5%以下，本研究開發合金材質食品器具中鉛與銻之檢驗方法。本研究挑選鑄鐵、鋁合金、黃銅及不鏽鋼等4種材質食品器具進行探討，前處理部分測試了研磨與剪小塊之取樣方式及不同酸組成對微波消化的影響，以及比較ICP-OES與ICP-MS之分析結果。經測試後，以檢體取樣效率較高之剪小塊方式取樣，加入王水進行微波消化，消化後之檢液再以ICP-MS進行分析。以0.1%及0.01%之鉛及銻進行4種金屬合金材質食品器具之添加回收試驗，鉛之回收率介於97.1-102.8%，變異係數介於0.2-3.2%；銻之回收率介於90.5-104.7%，變異係數介於0.4-8.6%，皆符合衛生福利部食品藥物管理署公布之食品化學檢驗方法之確效規範。另以鑄鐵、鋁合金、黃銅、易切黃銅及不鏽鋼之參考物質進行方法驗證，鉛及銻之測試值皆符合其標示值。本方法之定量極限，鉛與銻皆為0.01%。以所建立之檢驗方法評估市售8件金屬合金檢體之方法適用性，測試結果僅1件鋁合金檢體檢出鉛0.02%，其餘之鉛及銻均未檢出，皆符合法規標準。

The amendment of the“Sanitation Standard for Food Utensils, Containers and Packages“was announced by the Ministry of Health and Welfare on January 11, 2023, in which the metal alloys were divided into two categories:“metal alloy- the direct contact surface material with food is metal alloy”and“metal alloy- the direct contact surface material with food is synthetic resins.”The newly updated standards for the limits of lead (not more than 0.1%) and antimony (not more than 5%) were added to the material test of“metal alloy- the direct contact surface material with food is metal alloy.”This study developed an analytical method of lead and antimony in metal alloy food utensils and containers. Four materials of metal alloy food utensils were investigated in this study, including cast iron, aluminum alloy, copper, and stainless steel. For the sample preparation, the effects of grinding and cutting into small pieces with different acid treatment were tested, and the results of ICP-OES and ICP-MS analysis were also compared. According to the pretest result, samples cutting into small pieces showed higher preparation efficiency. The small sample pieces were digested in aqua regia using a microwave digester, and then analyzed by ICP-MS. The recovery tests were performed with 0.1% and 0.01% lead and antimony spiked in four types of metal alloy food utensils. The average recoveries of lead were between 97.1% and 102.8%, and the coefficients of variation were between 0.2% and 3.2%. The average recoveries of antimony were between 90.5% and 104.7%, and the coefficients of variation were between 0.4% and 8.6%. All results met the criteria outlined in the“Validation Guideline of Food Chemical Testing Methods”published by TFDA. This method was also certified using the standard reference materials (SRM) of cast iron, aluminum alloy, brass, easy-cutting brass, and stainless steel. The detected values of lead and antimony all met their labeled values. The limits of quantification (LOQs) were both 0.01% for lead and antimony. Eight commercial metal alloy food utensils were used to evaluate the applicability of this method. Only one aluminum alloy food utensil was detected with lead at 0.02%, and the others were not detected with lead and antimony, all of which complied with the sanitation standard.