Simultaneous Determination of Nine Components in Zhibaidihuang Concentrated Pills by HPLC-MS/MS
SUN Ying-guang1, 2, SHENG Ning1, ZHI Xu-ran1, YUAN Lin1, DU Ying-feng1, LIU Min1, YU Xiao-han1, ZHANG Lan-tong1*
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1.Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, Shijiazhuang 050017, China;2. Department of Pharmacy, Hebei General Hospital, Shijiazhuang 050051, China
OBJECTIVE To develop a method for the determination of neomangiferin, mangiferin, timosaponin BII, timosaponin AⅢ, berberine, morroniside, loganin, paeoniflorin, and paeonol in Zhibaidihuang concentrated pills(traditional Chinese medicine) by HPLC-MS. METHODS The samples were separated on a Diamonsil C18 column (4.6 mm×150 mm, 5 μm ) by gradient elution using acetonitrile and 0.1% aqueous formic acid as the mobile phase. The column temperature was 30 ℃. The elution program was optimized as follows: 0-2.5 min, linearly changed from A-B(5∶95, V/V) to A-B (55∶45, V/V); 2.5-5 min, linearly changed from A-B (55∶45, V/V) to A-B (95∶5, V/V); and 5-15 min, isocratic elution A-B (95∶5, V/V); then quickly returned to initial A-B (5∶95, V/V). This was followed by an equilibration period of 6 min prior to injection of next sample. The flow rate of mobile phase was set at 0.8 mL·min-1, and the injection volume was 10 μL. Multiple-reaction monitoring (MRM) scanning was employed for quantification with switching electrospray ion source polarity between positive and negative modes in a single run. RESULTS There was significant correlation between the peak area and concentration of each compound within the test range (r>0.999 3). The average recoveries (n=3) of the nine compounds were 98.33%, 99.73%, 100.1%, 101.2 %, 101.2%, 100.2%, 99.90%, 100.6% and 100.5%, respectively. The RSDs were 1.99%, 1.57%, 1.21%, 2.73%, 1.76%, 1.59%, 1.11%, 1.70% and 1.05%, respectively. CONCLUSION The method is simple, accurate and highly reproducible, and can be used for the determination of nine compounds in Zhibaidihuang concentrated pills.
SUN Ying-guang, , SHENG Ning, ZHI Xu-ran, YUAN Lin, DU Ying-feng, LIU Min, YU Xiao-han, ZHANG Lan-tong*.
Simultaneous Determination of Nine Components in Zhibaidihuang Concentrated Pills by HPLC-MS/MS[J]. Chinese Pharmaceutical Journal, 2014, 49(2): 152-155 https://doi.org/10.11669/cpj.2014.02.017
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