連翹十五成分之分離與確認   全文下載

Separation and Identification of the Fifteen Constituents in Forsythiae Fructus

連翹為常用中藥，是木樨科植物的乾燥種子，含有rengyoside B (1)、matairesinol (2)、salidroside (3)、quercitrin (4)、suspensaside (5)、rengyoside C (6)、matairesinoside (7)、forsythiaside (8)、pinoresinol-s-D-glucoside (9)、cornoside (10)、acteoside (11)、arctigenin (12)、arctiin (13)、phillyrin (14)及pinoresinol (15)等主要藥理活性成分。本文以磷酸鹽及甲醇-氰甲烷的緩衝溶液為沖提系統，在Cosmosil 5C18-ARII分離管柱，254及280 nm偵測波長及流速0.8 mL/min之線性梯度沖提程式下，可於60 min內完全分離連翹藥材中前述15個組成成分，各波峰經UV及MS確認。本分析方法僅需將磷酸鹽換成醋酸，就可應用於LC-MS分析。以重複六次注射計算其積分面積比值之相對標準偏差，同日在0.23~1.50%之間，隔日在0.41~2.40%之間。偵側極限為0.14~0.27 μg/mL。

Forsythiae Fructus, a commonly used Chinese herbal medicine derived from the dried seeds of Oleaceae plants, contains rengyoside B (1), matairesinol (2), salidroside (3), quercitrin (4), suspensaside (5), rengyoside C (6), matairesinoside (7), forsythiaside (8), pinoresinol-β-D-glucoside (9), cornoside (10), acteoside (11), arctigenin (12), arctiin (13), phillyrin (14) and pinoresinol (15) as its major bioactive constituents. In this study, a high performance liquid chromatography (HPLC) method using a Cosmosil 5C18-AR Π column, and a mixture of phosphate solution and methanol-acetonitrile as the mobile phase with detection of absorbance at 254 or 280 nm was developed to successfully resolve these 15 compounds within 60 min. Peaks were identified by matching the UV spectra and MS information with those of authentic standards or literature data. The method was applicable to LC-MS if the phosphate was replaced with an acetate solution. Calibration curves for 4 of the 15 constituents were obtained around a concentration range of 2 orders of magnitude and showed good linearity. The reproducibility (RSD) of the proposed method was 0.23-1.50% (intraday) and 0.41-2.40% (interday). The detection limits (S/N = 3) for the constituents were determined to be 0.16-0.27 μg/mL.