Simultaneous Determination of Eight Compounds in Shegan Mixtures by UHPLC-MS/MS / 中国药师

ABSTRACT

Objective:To establish an UHPLC-MS/MS method to determine the contents of baicalin,scutellarin,wogonin,caffeic acid,ephedrine,belamcandin,irisflorentin and baicalein in Shegan mixtures. Methods:The chromatographic separation was performed on a ZORBAX SB-C18 column(2. 1 mm × 50 mm,1. 8 μm)with the mobile phase consisting of acetonitrile and water(0. 1% formic acid),the flow rate was 0.3 ml·min-1,and the column temperature was 35℃. Electrospray ionization source(ESI)was used with multiple reaction monitoring( MRM)combined with positive and negative scanning switch. üegative ion mode detection was used for caf-feic acid,belamcandin and scutellarin ,while positive ion mode detection was used for baicalin,wogonin,irisflorentin,baicalein and e-phedrine. Results:The quantification limit of baicalin,scutellarin,wogonin,caffeic acid,ephedrine,belamcandin,irisflorentin and ba-icalein was 1. 44 × 10-4 ,4. 20 × 10-3 ,2. 95 × 10-4 ,7. 80,4. 90 × 10-3 ,4. 6 × 10-2 ,3. 18 × 10-4 ng·ml-1 and 4. 85 ng·ml-1 . The detection limit was 4.32 ×10-5,1.3 ×10-3,8.84 ×10-5,0.77,2.90 ×10-4,3.33 ×10-4,9.5 ×10-5 ng·ml-1 and 1.46 ng· ml-1 ,respectively. The correlation coefficients( R2 )were all higher than 0. 992 3 within the linear ranges. Both intra- and inter-day RSD were less than 5%. The average recoveries of the eight components were within the range of 80%-120%. Conclusion:The method is simple,rapid,sensitive and accurate. It can be used to determine the contents of baicalin,scutellarin,wogonin,caffeic acid,ephed-rine,belamcandin,irisflorentin and baicalein in Shegan mixtures for the quality control.