[关键词]
[摘要]
目的 采用高效液相-库仑阵列电化学法(HPLC-ECD)同时测定青天葵中鼠李柠檬素和鼠李秦素含量,并对不同培养方法及不同生长阶段的青天葵进行测定分析。方法 采用Agilent HC-C18色谱柱(150 mm×4.6 mm,5 μm),以甲醇∶乙腈(体积比2∶1)混合后加5 % 20 mmol·L-1 NaH2PO4(A)-20 mmol·L-1 NaH2PO4水溶液,用H3PO4调pH至2.50(B)为流动相,A∶B=48∶52等度洗脱,流速:1 mL·min-1,进样量15 μL,柱温:35 ℃,检测电压:50,150 mV。结果 鼠李柠檬素和鼠李秦素的线性范围分别为0.2~50.1 μg·mL-1(r=0.9999)和0.15~36.4 μg·mL-1(r=0.9999),平均回收率(n=9)分别为97.98 %(RSD=1.50 %)和97.64 %(RSD=2.49 %)。结论 HPLC-ECD法测定青天葵中鼠李柠檬素、鼠李秦素操作简便、准确,灵敏度高,不同培养阶段药材含有的鼠李柠檬素、鼠李秦的含量有一定差异,可为青天葵质量标准制定及提高提供依据。
[Key word]
[Abstract]
Objective To establish a method for simultaneous determination of rhamnocitrin and rhamnazin in Folium Nerviliae Fordii(FNF) with high performance liquid chromatography-electrochemical detection(HPLC-ECD),and to assay FNF cultivated with different methods and FNF at different growth stages. Methods The analytical method was carried out on an Agilent HC-C18 column(150 mm×4.6 mm,5 μm) with a mobile phase of methanol-acetonitrile(volume ratio being 2∶1) mixed with 5 % of 20 mmol·L-1 NaH2PO4(A)-20 mmol·L-1 NaH2PO4 aqueous solution with pH being 2.50 adjusted by H3PO4(B),The ratio A to B was 48∶52(A∶B), flow rate was 1.0 ml·min-1. The detection voltage was set at 50,150 mV,column temperature was 35 ℃,and the injection volume was 15 μL.Results The calibration curves were linear within the range of 0.2~50.1 μg·mL-1 for rhamnocitrin(r=0.9999) and 0.15~36.4 μg·mL-1 for rhamnazin(r=0.9999).The average recoveries(n=9)were 97.98 % for rhamnocitrin(RSD= 1.50 %) and 97.64 % for rhamnazin(RSD=2.49 %).Conclusion The contents of rhamnocitrin and rhamnazin in FNF vary in different growth stages. Electrochemical detection is convenient,accurate and sensitive,and it can be used for the upgrading of quality standard of FNF.
[中图分类号]
R284.1
[基金项目]
中柬第三方检测平台建设项目-2012年广州市白云区国际科技合作计划项目(2012-KQ-23)。