運用 LC-Q-TOF/MS 建立銀杏葉萃取物與白果仁之指紋圖譜及其在製劑上的應用   全文下載

Fingerprint Analysis of Ginkgo biloba Extract and Ginkgo semen in Preparations by LC-Q-TOF/MS

以超高效液相層析串聯四極桿／飛行式質譜儀（LC-Q-TOF/MS）的方法建立銀杏葉萃取物與白果仁之指紋圖譜。所有藥材與市售製劑檢體均以 70%甲醇萃取，再取部分萃取液進行水解。高效液相層析條件為：C18 管柱（3.0 × 150 mm, 2.7 μm），移動相為水和甲醇均含 0.01 % 的甲酸水溶液，混合溶液以流速 0.5 mL/min 梯度沖提。質譜條件選擇負離子模式，並以標準品及文獻之分子量比對確認，分別建立銀杏葉萃取物與白果仁水解前後的成分表，且於白果仁中發現銀杏內酯 J（Ginkgolide J）與白果內酯 （Bilobalide）為其他文獻未記載。本方法除了可區別銀杏葉萃取物與白果仁藥材成分的差異外，並可在未經水解之檢體鑑別出市售銀杏相關製劑含銀杏葉萃取物或白果仁，減少現行檢驗需經水解之時間，提升檢驗效率。"

An ultra-high performance liquid chromatography with tandem quadrupole/flight mass spectrometry (LC-Q-TOF/MS) method was developed for the chromatographic fingerprint analyses of Ginkgo biloba extract and Ginkgo semen. All samples were extracted with 70% methanol and part of each extract was hydrolyzed by acids. The chromatographic analyses of these materials were performed on a C18 analytical column (3.0 × 150 mm, 2.7 μm) with gradient elution using methanol and water with 0.01% formic acid at a flow rate of 0.5 mL/min. Mass spectrometry was performed in the negative-ion mode ESI to determine the compounds in G. biloba extract and G. semen by comparison with the accurate molecular weight of the reference compounds and literature reported. In addition, Ginkgolide J and Bilobalide were identified from G. semen by this method for the first time. The method was successfully used to analyze compounds in G. biloba extract and G. semen with significantly reduced analytical time, and also applied in the analysis of more complex components in G. biloba products.