高效液相色谱-电喷雾串联质谱法测定保健食品中水苏糖含量

Determination of Stachyose in Health Food by High Performance Liquid Chromatography/Mass Spectrometry

目的以质谱定性定量,测定保健品中水苏糖含量。方法采用高效液相色谱/电喷雾质谱联用法(HPLC-ESI/MS),色谱柱:瑞典KromasilNH2柱;流动相:甲醇+乙腈+0.1%甲酸氨水溶液=8+52+40(体积比);流速1.0ml/min。质谱采用电喷雾正离子模式(ESI+),对m/z689进行选择离子监测,扫描范围(m/z):620～700amu。结果水苏糖在80～120μg/ml范围内,峰面积和浓度呈良好的线性关系(r=0.9992);相对标准偏差(RSD)为0.73%;在3个添加水平下的回收率均在93.0%～105.8%。结论本方法快速、选择特异性高、分析时间短且无需衍生处理,抗干扰能力强,能准确快速测定水苏糖的含量。

Objective To develop a simple, rapid and accurate method to determine stachyose. Method A high performance liquid chromatography/eleetrospray ionization mass spectrometry （HPLC-ESI/MS） was used. The analyte of samples were separated on a Kromasil NH2 column with a ternary solvent mixture of methanol ＋ acetonitrile ＋ 0.1% water solution of ammonia formate （8 ＋52 ＋ 40, v/v/v） as the mobile phase at a flow rate of 1.0 ml/min. Stachyose was identified and quantified by electrospray ionization mass spectrometry （ESI-MS）, and the electrospray ionization was operated in positive ion mode to generate protonated ions. The ion at m/z 689 was recorded in the selective ionization and the scan range was 620-700 amu. Results The concentration of stachyose over a range of 80-120 μg/ml was in a good linearity. The correlation coefficient of the calibration curve was 0.999 2 and the RSD was 0.73% . The average recovery were between 93.0% and 105.8% . Conclusion The advantages of the proposed method are easy to operate without derivation and less time for analysis, and are in good precision and accuracy.