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原料「甲基硫醯基甲烷」中二甲基亞碸之檢驗方法

Method of Test for Dimethyl Sulfoxide in Methylsulfonylmethane as a Food Ingredient

摘要


衛生福利部108年10月18日公告修正,食品原料「甲基硫醯基甲烷(methylsulfonyl methane, MSM)」如以二甲基亞碸(dimethyl sulfoxide, DMSO)與過氧化氫(hydrogen proxide)合成,成品(係指甲基硫醯基甲烷原料)之二甲基亞碸殘留量需低於0.05%。本研究利用氣相層析儀搭配火焰離子檢出器(GC-FID)分析膠囊錠狀食品中DMSO殘留量,層析管柱使用DB-23毛細管(內膜厚度0.25 μm,內徑0.25 mm × 30 m),移動相為氦氣,流速1 mL/min,注入器溫度250℃,檢出器溫度300℃,分流比5:1。以二乙二醇一甲基醚(diethylene glycol methyl ether, DGME)作為內部標準品,前處理以丙酮為萃取溶劑,於室溫超音波振盪20分鐘。確效結果顯示,於空白基質中分別添加0.05及0.1% DMSO之平均回收率為94.8及96.9%,變異係數為0.92及0.95%,符合食品化學確效規範;本檢驗方法之定量極限為0.01%。以所建立之方法應用於14件市售膠囊與錠狀食品中DMSO含量檢測,結果均為未檢出。

並列摘要


The residue of dimethyl sulfoxide (DMSO) in methylsulfonylmethane (MSM) as a food ingredient should be lower than 0.05% according to the MOHW regulation. This study aimed on the rapid determination of DMSO residue in MSM by gas chromatograph coupled with a flame ionization detector (GC-FID). Chromatography was performed on a capillary column DB-23 (30 m × 0.25 mm i.d., 0.25 μm film thickness). Helium carrier gas flow rate was set at 1 mL min^(-1). Injector temperature was set at 250°C with a split injection of 5:1. Detector temperature was set at 300°C. DMSO in samples was extracted by acetone for 20 minutes in an ultrasonic bath. Diethylene glycol methyl ether (DGME) was selected as an internal standard for the accurate quantification of DMSO in samples. Accuracy was conducted by spiking 0.05 and 0.1% DMSO into the blank samples, and the obtained average recoveries were 94.8 and 96.9%, and the coefficients of variation were 0.92 and 0.95%, respectively. The limit of quantification was estimated to be 0.01%. The surveillance results of 14 commercial food samples purchased form demotic market showed that DMSO was not detected in all of them.

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