高效液相色谱质谱联用法同时测定金莲清热颗粒中荭草苷、知母皂苷等7种成分的含量

Simultaneous Determination of Seven Components in Jinlianqingre Granules by HPLC-MS

目的建立HPLC-MS测定金莲清热颗粒中荭草苷、牡荆苷、金丝桃苷、新芒果苷、芒果苷、知母皂苷BⅡ和知母皂苷AⅢ7种成分含量的方法。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。结果金莲清热颗粒中7种成分峰面积与浓度呈良好的线性关系,r>0.999 2;加样回收率分别为99.34%,99.28%,101.6%,101.3%,100.5%,101.9%和98.86%(n=3)。RSD值分别为1.12%,1.36%,1.57%,1.74%,1.52%,1.43%和0.92%。结论该方法简便,准确,重现性好,专属性高,可用于金莲清热颗粒的质量控制。

OBJECTIVE To develop a method for the determination of orientin, vitexin, hyperin, neomangiferin, mangiferin,timosaponin BII and timosaponin A m in Jinlianqingre granules（ traditional Chinese medicines） by HPLC-MS. METHODS The samples were separated on a Diamonsil Cls column （4. 6 mm × 150 mm, 5 μm ） by gradient elution using acetonitrile and 0. 1% aqueous formic acid as the mobile phase at a flow rate of 800 μL · min-1. The column temperature was 30 ℃. 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 Complete separation was obtained within 15 min for the seven compounds. The regression equations showed linear relationships between the peak area and content of each compound （ r 〉 0. 999 2）. The average recoveries of the com- pounds listed above were 99.34% , 99. 28% , 101.6%, 101.3% , 100. 5% , 101.9% and 98. 86% （ n = 3）, and the RSDs were 1.12%, 1.36%, 1.57%, 1.74%, 1.52%, 1.43% and 0. 92%, respectively. CONCLUSION The method is simple, accurate and highly reproducible, and can be used for the determination of seven compounds in Jinlianqingre granules.