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DiamonsilC18柱(4.6mm×150mm,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>0.9992;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。
Abstract
OBJECTIVE To develop a method for the determination of orientin,vitexin,hyperin,neomangiferin,mangiferin,timosaponin BII and timosaponin AⅢ in Jinlianqingre granules(traditional Chinese medicines) 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 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 compounds 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.
关键词
高效液相色谱质谱联用法 /
金莲清热颗粒 /
荭草苷 /
牡荆苷 /
芒果苷 /
知母皂苷BⅡ /
含量测定
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Key words
HPLC-MS /
Jinlianqingre granule /
orientin /
vitexin /
mangiferin /
timosaponin BⅡ /
content determination
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中图分类号:
R284
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参考文献
Ch.P (2010) VolⅠ(中国药典2010年版.一部) ,2010: 829. FANG H M,HAN R X,LIU X F, et al.Detection of sarsasapogenin in Jinlianqingre granule by RP-HPLC .Acta Acad Med Nei Mongol (内蒙古医学院学报),2008,30(6):516-518. DING J B,LI Y P,ZHANG J M,et al.Assay of sarsasapogenin in Jinlianqingre Capsules by thin layer scanning chromatography . Ningxia Med J (宁夏医学杂志),2003,25(5):274-276. XU X J,XIE B X,LI Z M.Determination of indirubin in Jinlianqingre effervescent tablets by HPLC . Strait Pharm J (海峡药学),2011,23(2):39-40. LIN Q F,FENG S Q,LI Y L,et al.Study on the antibacterial and antiviral activity compositions of Trollius chinensis Bunge .J Zhejiang Univ( Sci Ed),2004,31(4):412-415. SUN Y G,DU Y F,LIU Y,et al.Simultaneous determination of 9 components in Anemarrhena asphodeloides by liquid chromatography-tandem mass spectrometry combined with chemometric techniques . J Sep Sci,2012,35:1796-1807.
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脚注
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基金
2012年河北省自然科学基金-石药集团医药联合研究基金(H2012206079)
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