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膠囊錠狀食品及茶包中sennosides檢驗方法之探討

Determination of Sennosides in Teabags and Foods in Capsule or Tablet form by HPLC/PDA

摘要


本研究建立以高效液相層析法搭配光二極體陣列檢測器(HPLC/PDA),分析含番瀉葉之膠囊錠狀食品及茶包食品中sennosides含量之方法。膠囊錠狀食品與茶包檢體分別經70%甲醇溶液及去離子水萃取過濾後,採用C18層析管柱,以乙腈及0.085%磷酸溶液為移動相溶液進行梯度沖提,利用高效液相層析儀於波長270 nm進行分析。sennoside A (濃度0.16-81.7 μg/mL)及sennoside B (濃度0.16-83.45 μg/mL)標準曲線之線性關係良好,其判定係數(r^2)均於0.999以上。同日內與異日間試驗之相對標準偏差(RSD)分別為0.07-2.52%及0.10-1.30%。添加回收試驗結果:sennoside A回收率為107-108%,sennoside B回收率為99-104%,其相對標準偏差(RSD)分別小於2.30及2.38%。錠劑及茶包之偵測極限分別為0.53及0.27 μg/mL,而定量極限分別為1.77及0.80 μg/mL。應用本方法進行市售來源及組成均不同之17件檢體中sennosides含量分析,僅1件檢體之層析圖譜仍見些微干擾,針對該檢體進行個別調整後,亦可成功分離之,其餘檢體之層析圖譜均無干擾之情形,本方法將公開供各界進行sennosides檢測之參考。

並列摘要


A method for the analysis of sennosides in teabags and foods in capsule or tablet form by high performance liquid chromatography/photodiode array detector (HPLCIPDA) was developed. Metlianol (70%) and hot water (95°C) was applied for the extraction of sennosides from foods and teabags, respectively. The extracts were analyzed by HPLCIPDA system consisted of C18 reverse column and gradient mobile phase of acetonitrile and 0.085% H3P04 • The detection wavelength was 270 mu. The method demonstrated good linearities of sennoside A (range: 0.16-81.7 ug/m.l.) and sennoside B (range: 0.16-83.45 ug/ml.) with regression coefficients (r') all above 0.999. The recovery studies were conducted by spiking sennosides into sample extract at tlie concentration of 8.17-25.04 ug/ml.. For sennoside A, the average recoveries, relative standard deviations (RSDs) of intraday and interday recovery studies, limit of detection (LOD), and limit of quantification (LOQ) were 107-108%, 0.07-2.52%, 0.53 ug/ml., and 1.77 ug/ml. respectively. For sennoside B, the average recoveries, RSDs of intraday and interday recovery studies, LOD, and LOQ were 99-104%, 0.10-1.30%, 0.27 ug/ml., and 0.8 ug/ml. respectively. The method selectivity was tested in 17 commercial products. The results showed only 1 sample revealed a chromatographic interference which was further improved after manual adjustment. This report will provide as reference to administrative authorities and public.

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