膠囊錠狀食品中辛弗林檢驗方法研究   全文下載

Determination of Synephrine in Foods in Tablet and Capsule Form

辛弗林（synephrine）是一種生物鹼，天然存在於柑橘類植物，尤其在苦橙（bitter orange, Citrus aurantium）中為主要且具活性之物質。辛弗林因結構與被禁用之麻黃素類似，故取而代之並常用於減肥及增強運動表現的膳食補充品。衛生福利部針對苦橙中辛弗林於102年訂有食用限量，爰擬建立膠囊錠狀食品中辛弗林之檢驗方法，以供各界參考。本研究將均質樣品添加去離子水以超音波振盪萃取後，以超高效液相層析儀搭配光二極體陣列檢出器進行分析，採用分析管柱為Pursuit 5 PFP（4.6×150 mm, 5μm），定量波長為220 nm。於自製類似膠囊基質之空白樣品中分別添加p-辛弗林（p-synephrine）及m-辛弗林（m-synephrine）各5、25及50 mg／100 g進行確效試驗，結果顯示p-辛弗林及m-辛弗林之同日間回收率範圍分別為90.6－103.8％及88.5－103.0％，變異係數範圍分別為0.40－3.77％及1.27－6.41％，異日間回收率範圍分別為92.7－101.3％及89.5－98.7％，變異係數分別為1.43－3.57％及1.63－6.51％，符合食品藥物管理署食品化學檢驗方法之確效規範要求。繼而檢測網路販售商品計10件，p-辛弗林檢測範圍為低於定量極限至6487 mg／100 g，m-辛弗林檢測範圍為低於定量極限至164 mg／100 g，有3件產品之建議攝食量超過衛生福利部公告之每日食用限量，其中超量最高者達約5倍，顯示此類產品需加強查察其攝取量是否符合現行規範，不合格產品均已移請相關權責單位進行後續查處，以維護國人健康。

Synephrine is a predominant active alkaloid found in bitter orange (Citrus aurantium) fruit, as well as in other citrus species. It is similar in structure to ephedrine, which is banned in dietary supplements for weight loss and sport performance. The Ministry of Health and Welfare amounted the daily synephrine intake in bitter orange in 2013, while there was no corresponding test method published yet. Therefore, this study aimed at the development of a determination method for testing synephrine in foods by using ultra-performance liquid chromatography (UPLC) with photodiode array detection (PDA). Sample was ground to fine powders and extracted with ultrasonic assistant. The separation was done by using the UPLC system with an Agilent Pursuit 5 PFP column (4.6 mm × 15 cm, 5 μm) and connected to a photodiode array detector. The quantitative wavelength was set at 220 nm. The method validation was performed by spiking blank samples with p-synephrine and m-synephrine at the levels of 5, 25 and 50 mg/100 g. The average recoveries of p-synephrine and m-synephrine for intra-day analysis were 90.6 - 103.8% and 88.5 - 103.0% with coefficients of variation 0.40 - 3.77% and 1.27 - 6.41%, respectively. The average recoveries of p-synephrine and m-synephrine for inter-day were 92.7 - 101.3% and 89.5 - 98.7% with coefficients of variation 1.43 - 3.57% and 1.63 - 6.51%, respectively. The results showed that the method offered high precision and accuracy. The surveillance results consisted of ten commercial foods in capsule and tablet form showed that three samples exceeded the limit of daily synephrine intake. One of the violate sample contained synephrine five times higher than the regulation limit. All the illegal products had reported to relative authorities for further administration.