目的 建立一测多评法测定半夏Pinellia ternate及其混伪品天南星Arisaema erubescens、水半夏Typhonium flagelliforme和虎掌南星Pinellia pedatisecta中尿苷、腺嘌呤、鸟苷及腺苷的含量方法。方法 利用高效液相色谱法,采用Shim-pack Scepter C₁₈-120色谱柱(250 mm×4.6 mm,5 μm);流动相10%乙腈-水,梯度洗脱;体积流量1 mL/min;检测波长260 nm;柱温20℃。以腺苷为内标,建立尿苷、腺嘌呤和鸟苷的相对校正因子,同时采用外标法和一测多评法测定多批次药材中4种成分的含量,验证一测多评法的准确性和可行性。结果 尿苷、腺嘌呤、鸟苷及腺苷在各自线性范围内线性关系良好(r>0.999 9),平均加样回收率95.40%~104.02%,一测多评法和外标法测得的含量无显著差异(RSD<3%),不同产地的半夏中4种核苷含量显示有明显差异。除天南星外,基于核苷的含量测定结果结合化学计量分析可以很好地区分半夏、水半夏和虎掌南星。结论 该方法简便准确度高,可为半夏的质量控制和评价提供参考。

Objective To establish a method for the determination of uridine,adenine,guanosine and adenosine inPinellia ternate and its adulterants,includingArisaema erubescens,tubers ofTyphonium flagelliforme andPinellia pedatisecta by quantitative analysis of multi-components by a single marker (QAMS).Methods The nucleosides were analyzed in Shim-pack Scepter C₁₈-120 column (250 mm×4.6 mm,5 μm) by high performance liquid chromatography (HPLC);The gradient elution was carried out with the mobile phase composed of 10% acetonitrile-water at the flow rate of 1 mL/min and the detection wavelength of 260 nm,column temperature at 20℃.Adenosine was used as the internal reference substances to establish the conversion factors of uridine,adenine and guanosine.At the same time,the contents of multiple batches of medicinal materials were determined by external standard method and QAMS to verify the accuracy and feasibility of QAMS.Results The results showed that uridine,adenine,guanosine and adenosine had good linear relationship in the ranges of the tested concentrations (r>0.999 9),and the average recoveries were 95.40%-104.02%.There was no significant difference in the contents of uridine,adenine,guanosine and adenosine measured by QAMS and external standard method (RSD<3%).The contents of four kinds of nucleosides inPinelliae Rhizoma from different habitats showed significant variations.Except forArisaematis Rhizoma,Pinelliae Rhizoma,tubers ofT.flagelliforme andP.pedatisecta could be distinguished by the content of nucleoside combined with chemometrics.Conclusion The method has high accuracy and simple,which can provide a reference for the quality evaluation and control ofPinelliae Rhizoma.

R286.2

国家自然科学基金重点项目(82130111);国家自然科学基金青年项目(82003940)