高效液相色谱串联质谱法同时测定知柏地黄丸中新芒果苷等9种成分的含量  

Simultaneous Determination of Nine Components in Zhibaidihuang Concentrated Pills by HPLC-MS/MS

作　　者：孙颖光[1,2] 生宁[1] 支旭然[1] 苑霖[1] 杜英峰[1] 刘敏[1] 于小涵[1] 张兰桐[1] 

机构地区：[1]河北医科大学药学院药物分析教研室,石家庄050017 [2]河北省人民医院药学部,石家庄050051

出　　处：《中国药学杂志》2014年第2期152-155,共4页Chinese Pharmaceutical Journal

基　　金：河北省自然科学基金-石药集团医药联合研究基金(H2012206079)

摘　　要：目的建立高效液相色谱串联质谱法测定知柏地黄浓缩丸中新芒果苷,芒果苷,知母皂苷BⅡ,知母皂苷AⅢ,小檗碱,莫诺苷,马钱苷,芍药苷和丹皮酚含量的方法。方法采用Diamonsil C18柱(4.6 mm×150 mm,5μm);柱温30℃;乙腈-0.1%甲酸水溶液为流动相,以800μL·min-1梯度洗脱;质谱条件:采用电喷雾离子源正负离子模式同时进行检测,多反应监测模式(MRM)用于定量测定。结果知柏地黄丸中9种成分峰面积与浓度呈良好的线性关系,在15 min内知柏地黄丸中9种成分峰面积与浓度线性关系良好,r>0.999 3;加样回收率(n=3)分别为98.33%,99.73%,100.1%,101.2%,101.2%,100.2%,99.90%,100.6%和100.5%。RSD值分别为1.99%,1.57%,1.21%,2.73%,1.76%,1.59%,1.11%,1.70%和1.05%。结论该方法简便,准确,重现性好,专属性高,可用于知柏地黄丸的质量控制。OBJECTIVE To develop a method for the determination of neomangiferin, mangiferin, timosaponin BII, timosaponin A m, berberine, morroniside, loganin, paeoniflorin, and paeonol in Zhibaidihuang concentrated pills （traditional Chinese medicine ） by HPLC-MS. METHODS The samples were separated on a Diamonsil Cls column （4. 6 mmx 150 ram, 5 p.m ） by gradient elution using acetonitrile and 0. 1% aqueous formic acid as the mobile phase. The column temperature was 30 ~C. The elution program was optimized as follows： 0 -2. 5 rain, linearly changed from A-B （5： 95, V/V） to A -B （55： 45, V/V） ; 2. 5 -5 rain, linearly changed from A-B （55：45, V/V） to A -B （95：5, V/V） ; and 5 -15 rain, 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 rain prior to injection of next sample. The flow rate of mobile phase was set at 0. 8 mL ~ rain-I , and the injection volume was 10 p.L. 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.

关 键 词：液质联用 知柏地黄丸 含量测定 新芒果苷 芒果苷 

分 类 号：R917[医药卫生—药物分析学]