膠囊錠狀食品中甲基硫醯基甲烷之檢驗方法   全文下載

Method of Test for Methylsulfonylmethane in Foods in Tablet and Capsule Form

甲基硫醯基甲烷（Methylsulfonylmethane, MSM）為天然存在之含硫有機成分，可單獨或配合葡萄糖胺、軟骨素及膠原蛋白等成分常見於保健食品中。衛生福利部102年9月2日公告修正，原料「甲基硫醯基甲烷」之每日食用限量為6公克，且單一次劑量不得超過2公克。本研究利用氣相層析儀搭配火焰離子檢出器（GC／FID）進行分析，層析管柱使用DB-23毛細管（內膜厚度0.25μm，內徑0.25 mm×30 m），載氣為氦氣，流速1 mL／min，注射進樣溫度250℃，檢出器溫度300℃，分流比25：1。以乙二醇二甲基醚（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5分鐘，適用範圍包括膠囊錠狀之樣品基質。確效結果顯示，於空白基質中添加100及500 mg／g MSM之平均回收率為95.8及93.5％，變異係數為5.50及0.38％，符合食品化學檢驗方法確效規範；本檢驗方法之定量極限為5 mg／g。15件市售膠囊與錠狀食品中MSM之含量檢測結果，檢測值與標示值之百分比除2件分別為32.0及46.3％外，其餘13件均介於81.5－101.5％；15件之每日建議使用量均未超出法規訂定之每日使用限量。

Methylsulfonylmethane (MSM), an organic sulfur-containing compound, is either alone or in combination with glucosamine in dietary supplements commonly. The recommended maximum level of daily intake of MSM promulgated in 2013 by the Ministry of Health and Welfare was 6 g/day and 2 g for a single-dose. This study aimed on using a gas chromatograph with a flame ionization detector (GC–FID) for the rapid assay of methylsulfonylmethane (MSM) contents in foods in tablet or capsule form. 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 0.7 mL min-1. Injector temperature was set 250°C with a split injection of 25:1. Detector temperature was set 300°C. MSM was extracted with acetone for 5 min in an ultrasonic bath. Diethylene glycol methyl ether was selected as an internal standard for the accurate quantitation of MSM in samples. Accuracy was evaluated by spiking 100 and 500 mg/g MSM into blank samples. The average recoveries were 93.5 and 95.8%, and their coefficients of variation were 0.38 and 5.50%, respectively. The limit of quantitation was estimated to be 5 mg/g. The surveillance results of 15 commercial food samples in the market were as follows: two of the samples contained 32.0 and 46.3% of the labeled value in the package, and the other 13 samples contained MSM between 81.5-101.5% of the labeled value. The labeled daily consumption values of MSM in the 15 samples did not exceed the recommended daily intake of the regulation.