橘黴素檢測方法確效及不確定度評估

Assessed by uncertainty and validated on detection method for citrinin

彭文伸(Wun-Shen Peng)

指導教授 ： 陳齊聖

朝陽科技大學/理工學院/應用化學系生化科技碩博士班/碩士(2015年)

摘要

近年來養生觀念崛起，食用紅麴食品以及保健食品的人口增加，其相
關產品種類繁多，然而紅麴菌二次代謝物會產生，具有保健功效的產物，亦會產生具有強烈腎毒性的橘黴素，因此造成人們食入橘黴素風險也跟著增加。本研究以固液萃取法，以及液相層析串聯式質譜儀，建立分析方法，
並進行方法確效與方法不確定評估。實驗結果檢量線線性範圍為0.5-500 ng/mL、迴歸係數0.9989，檢出限量為20 ng/mL (S/N ≥10)。準確度及精密度測試，將添加濃度20、40、2000 ng/mL橘黴素標準品，分別添加入各類檢體中。實驗結果準確度測試各檢體之回收率，分別為玉米檢體78.00%-110.00%、紅麴餅乾檢體72.00%-95.00%、米檢體79.84%-116.00%、燕麥檢體72.00%-118.00%。各類檢體精密度試驗結果，重覆性試驗結果各檢體變異係數，都小於10，中間精密度變異係數分析結果，除了玉米、燕麥檢體添加濃度20 ng/mL變異係數高於10%，其餘分析結果變異係數皆小於10%。各檢體之擴充不確定度評估結果，玉米3922±386.08 ng/mL、紅麴餅乾3922±310.24 ng/mL、米4018±483.50 ng/mL、燕麥3922±460.60 ng/mL。

關鍵字

固液萃取法 ； 液相層析串聯式質譜儀 ； 橘黴素 ； 確效

並列摘要

In recent years, due to health concerns, red kojic rice has drawn a lot of attentions. A wide variety of red kojic rice related products are being sold on the market. Monascus purpureus is the fermenting mold for making red kojic rice and its secondary metabolites has been shown to provide health benefits. However, the mold also produces citrinin that exhibits strong nephrotoxicity, leading to health risks. In this study, we used solid-liquid extraction and LC-MS/MS to establish an analytical method, and assessed the uncertainty and validation of the method. Experiment results showed that the calibration curve linear range of 0.5-500 ng/mL, the regression coefficient was 0.9989, and the detection limit was 20 ng/mL (S/N≥10). Accuracy and precision of tests were run, for 20, 40 and 2000 ng/mL citrinin standards concentrations added to various types of samples. The recoveries for each specimen were 78.00%-110.00% for corn, 72.00%-95.00% for red kojic rice crackers, 79.84%-116.00% for rice, and 72.00%-118.00% for oat. Among repetitive tests, the coefficient of variation was less than 10%. In the intermediate precision coefficient of variation analysis, the variation higher than 10% for corn (20 ng/mL citrinin added), the remaining results were all less than 10% coefficient of variation. The assessment of expansion uncertainties were 3922±386.08 ng/mL for corn, 3922±310.24ng/mL red kojic rice crackers, 4018±483.50 ng/mL for rice, and 3922 ±460.60 ng/mL for oat.

並列關鍵字

Solid-liquid extraction ； LC-MS/MS ； Citrinin ； Validation

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