HPLC-ESI-MS联用法测定保健品中荷叶碱的含量

[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(5μm,4.6 mm×250.0 mm);流动相,A:0.1%三乙胺水溶液,B:乙腈,梯度洗脱;检测波长278 nm。[结果]荷叶碱在0.17~21.20μg/ml浓度范围内线性关系良好,r=0.999 6;最低检测限为0.01μg/ml(S/N=3);最低定量限为0.30μg/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。

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

[Objective] The aim of this paper was to establish a high performance liquid chromatography-electrospray mass spectrometry(HPLC-ES/MS)method to determine nuciferine.[Method] Column was Spherigel-C-18 column(5 μm,4.6×250.0 mm).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 μg/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 μg/ml(S/N=3).Quantifition minimum was 0.30 μg/ml(S/N=10).[Conclusion] The proposed method had the advantages of easy operation,without derivation,less analysis time,good precision and accuracy.