Objective: The purpose of this study was to develop a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the determination of the contents of polygalaxanthone Ⅲ and 3

6'-disinapoyl sucrose. Method: Separation was performed on ZORBAX Eclipse plus C18 column(4.6 mm×100 mm

3.5 μm) with the following settings:mobile phase cetonitrile-0.1% formic acid (28:72);flow rate 0.3 mL·min-1;the injection volume 10 μL;column temperature 20 ℃. MS condition

electrospray ionization (ESI) and multiple reaction monitoring (MRM) were adopted. The most abundant precursor/production pairs were m/z 567.2-345.1 for polygalaxanthone Ⅲ

and m/z 753.3-205.1 for 3

6'-disinapoyl sucrose. Result: The two components showed good linearity and the analyzing process was just within 6 min. The intra-day precision and inter-day precision for polygalaxanthone Ⅲ were 2.2% and 2.5% respectively;the recoveries were between 96.1% and 101.7% with RSD 2.4%.While the intra-day precision and inter-day precision for 3

6'-disinapoyl sucrose were 2.3% and 2.4%;the average recoveries were in the range of 95.7%-101.4% with RSD 2.0%. Conclusion: The method is rapid

sensitive

selective and suitable for the quantitative analysis of polygalaxanthone Ⅲ and 3

6'-disinapoyl sucrose in polygala tenuifolia.