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

孙颖光,杜英峰,生宁,苑霖,于小涵,刘敏,张兰桐

中国药学杂志 ›› 2013, Vol. 48 ›› Issue (16) : 1407-1411.

中国药学杂志 ›› 2013, Vol. 48 ›› Issue (16) : 1407-1411. DOI: 10.11669/cpj.2013.16.019
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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

  • 孙颖光12,杜英峰1,生宁1,苑霖1,于小涵1,刘敏1,张兰桐1
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Simultaneous Determination of Seven Components in Jinlianqingre Granules by HPLC-MS

  • SUN Ying-guang1,2,DU Ying-feng1,SHENG Ning1,YUAN Lin1,YU Xiao-han1,LIU Min1,ZHANG Lan-tong1
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摘要

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

Key words

HPLC-MS / Jinlianqingre granule / orientin / vitexin / mangiferin / timosaponin BⅡ / content determination

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孙颖光,杜英峰,生宁,苑霖,于小涵,刘敏,张兰桐. 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[J]. 中国药学杂志, 2013, 48(16): 1407-1411 https://doi.org/10.11669/cpj.2013.16.019
SUN Ying-guang,,DU Ying-feng,SHENG Ning,YUAN Lin,YU Xiao-han,LIU Min,ZHANG Lan-tong. Simultaneous Determination of Seven Components in Jinlianqingre Granules by HPLC-MS[J]. Chinese Pharmaceutical Journal, 2013, 48(16): 1407-1411 https://doi.org/10.11669/cpj.2013.16.019
中图分类号: R284   

参考文献

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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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