高效液相色谱法测定两面针药材中2种成分含量

Content Determination of Two Components in Zanthoxylum Nitidum by HPLC

目的建立测定两面针药材中2种成分含量的高效液相色谱(HPLC)法。方法采用HPLC法测定不同来源(野生、栽培、药材市场)两面针药材样品(根、茎)中氯化两面针碱和白屈菜红碱成分含量,色谱柱为ThermoBETASILC_(18)柱(250 mm×4.6 mm,5μm),流动相为含0.2%三乙胺的0.3%磷酸溶液-乙腈(77∶23,V/V),流速为1.0 mL/min,检测波长为273 nm,柱温30℃,进样量10μL。结果氯化两面针碱、白屈菜红碱进样量分别在0.0182~1.138μg(r=0.9999,n=5)和0.0139~0.868μg(r=0.9999,n=6)范围内与峰面积线性关系良好;精密度、稳定性、重复性试验的RSD均小于2.2%;平均加样回收率分别96.30%和94.07%,RSD分别为1.15%和1.31%(n=6)。21批药材样品中氯化两面针碱和白屈菜红碱总含量为0.068%~0.395%,限度条件为两者总含量不得少于0.150%。结论该方法简单、可行,能有效评价两面针根及茎的质量,可为两面针药用部位的增加及资源可持续开发利用提供参考。

Objective To establish a high-performance liquid chromatography(HPLC)method for the content determination of two components in Zanthoxylum nitidum.Methods HPLC method was used to determine the contents of nitidine chloride and chelerythrine in Zanthoxylum nitidum samples(roots and stems)from different sources(wild,cultivated and marketed).The chromatographic column was Thermo BETASIL C_(18) column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.3%phosphoric acid solution containing 0.2%triethylamine(23∶77,V/V),the flow rate was 1 mL/min,the detection wavelength was 273 nm,the column temperature was 30℃,and the injection volume was 10μL.Results The linear ranges of nitidine chloride and chelerythrine were 0.0182-1.138μg(r=0.9999,n=5)and 0.0139-0.868μg(r=0.9999,n=6),respectively.The RSDs of precision,stability and repeatability tests were less than 2.2%.The average recoveries of nitidine chloride and chelerythrine were 96.30%and 94.07%with RSDs of 1.15%and 1.31%(n=6),respectively.The total content of nitidine chloride and chelerythrine in 21 batches of samples was 0.068%-0.395%,and the limit condition was that the total content of both should not be less than 0.150%.Conclusion The method is simple and feasible,and can effectively evaluate the quality of roots and stems of Zanthoxylum nitidum,so as to provide a reference for the increase of medicinal parts of Zanthoxylum nitidum and the sustainable development and utilization of resources.