不同部位和不同产地加工方法的知母质量评价研究

Quality evaluation of Anemarrhenae Rhizoma for different parts and different processing methods

目的采用UPLC-QQQ-MS/MS法同时测定不同部位和不同产地加工方法知母Anemarrhenae Rhizoma中9个成分的含量,并比较其差异。方法采用Waters ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7μm),流动相为0.01%甲酸溶液(A)-乙腈(B),梯度洗脱,体积流量0.4 mL/min,进样量2μL,柱温30℃;质谱采用电喷雾离子源、负离子模式(ESI-),多反应监测(multiple reaction monitoring,MRM)。结果知母中新芒果苷、芒果苷、异芒果苷、知母皂苷AⅡ、知母皂苷AⅢ、知母皂苷BⅡ、知母皂苷BⅢ、知母皂苷E1、知母皂苷Ⅰ 9个成分在各自范围内呈良好的线性关系,加样回收率97.23%~100.76%。知母的5个不同部位中知母须根中芒果苷、异芒果苷的含量最高;知母肉中知母皂苷E1、知母皂苷BⅡ、知母皂苷Ⅰ含量最高;知母头与知母片、知母肉成分差异较小。比较知母的不同产地加工方法,趁鲜切片新芒果苷和知母皂苷BⅡ的含量较高,润切片芒果苷和知母皂苷AⅢ的含量较高。结论知母须根具有一定的开发利用价值,知母肉具有其存在的合理性;知母产地加工,可不切去知母头,以减少工序,提高知母根茎的综合利用率;趁鲜切片可加速干燥,降低饮片霉变风险。

Objective To determine the contents of 9 components in Anemarrhenae Rhizoma for different parts and different processing methods by UPLC-QQQ-MS/MS method,and compared the differences. Methods The sample were separated on an Waters ACQUITY UPLC BEH C18 column(100 mm × 2.1 mm,1.7 μm), the mobile phase composed of 0.01% formic acid solution(A)-acetonitrile(B) with gradient elution.the flow rate was 0.4 mL/min and the injection volume was 2 μL.The column temperature was 30 ℃. Multiple-reaction monitoring(MRM)scanning was employed for quantification in negative ion mode under electrospray ion. Results The nine components(neomangiferin, mangiferin, isomangiferin, timosaponin E1,timosaponin BⅡ,timosaponin BⅢ,anemarrhenasaponin I,timosaponin AⅡ and timosaponin AⅢ) all showed good linear relationship in their respective ranges,the average recoveries of 9 components were 97.23%-100.76%.Among the five different parts of Anemarrhenae Rhizoma,the contents of mangiferin and isomangiferin were the highest in the fibrous root of Anemarrhenae Rhizoma, the contents of timosaponin E1,timosaponin BⅡ and anemarrhenasaponin I in Anemarrhenae Rhizoma with outer cork removed(called zhimurou) were the highest,there was little difference in the components among the apex in rhizome of Anemarrhenae Rhizoma(called zhimutou),Anemarrhenae Rhizoma pieces and zhimurou. Compared the different habitat processing methods of Anemarrhenae Rhizoma, the content of neomangiferin and imosaponin BⅡ were higher in fresh-cut slices, while the content of mangiferin and timosaponin AⅢ were higher in traditional-cut slices. Conclusion The fibrous root of Anemarrhenae Rhizoma is valuable in development and utilization, and the existence of zhimurou is rational. Zhimutou can be reserved in the habitat processing of Anemarrhenae Rhizoma in order to reduce the working procedure and improve the comprehensive utilization rate of the rhizome of Anemarrhenae Rhizoma.Fresh-cut slices can accelerate drying and reduce the risk of mildew.