HPLC-ESI-MS联用法测定保健品中荷叶碱的含量

Determination of Nuciferine Content in Health Food by HPLC-ESI/MS

[目的]建立含荷叶碱类保健食品中高效液相色谱-电喷雾质谱（HPLC-ESI/MS）检测方法。[方法]色谱柱为Spherigel-C-18柱（5um，4．6mm×250．0mm）；流动相，A：0．1％三乙胺水溶液，B：乙腈，梯度洗脱；检测波长278nm。[结果]荷叶碱在0．17～21．20ug／ml浓度范围内线性关系良好，r=0．9996；最低检测限为0．01ug/ml（S／N=3）；最低定量限为0．30ug/ml（S／N=10）；3种样品的平均回收率为96．66％-98．57％，RSD≤2．52％。[结论]该方法具有流动相简单、分析时间短，且不要对样品进行衍生，操作简便，定量准确，抗干扰能力强等优点。

[ Objective] The aim of this paper was to establish a high performance liquid chromatography-electrospray moss spectrometry （HPLC-ES/MS） method to determine nuciferine. [ Method ] Column was Spherigel- C- 18 column（ 5 pan, 4.6 × 250.0 nm）. The mobile phases was 0.1% N（ C2H5 ）3 （ A ） - acetonitrile （ B ）, gradient elution. The UV detector was at 278 nm. [ Result ] The calibration curves were linear in the ranges 0.17 - 21.20 ug/ml for nuciferine （ r =0.999 6） .The average recovery rate was 96.66% - 98.57%, RSD≤2.52% （ n = 3） .Determination minimum was 0.01 ug/ml（ S/ N = 3）. Quantifition minimum was 0.30ug/ml（ S/N = 10）. [ Conclusion] The proposed method had the advantages of easy operation, without derivation, less analysis time,good precision and accuracy.