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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 qualitative and quantitative by mass spectrometry, determination of stachyose content in health care products. Methods The HPLC-ESI / MS method was used. The column was Kromasil NH2 column. The mobile phase consisted of methanol + acetonitrile + 0.1% formic acid in ammonia solution = 8 + 52 + 40 by volume. Flow rate 1.0 ml / min. Mass spectrometry Selected ion monitoring of m / z 689 using electrospray positive ion mode (ESI +) with scan range (m / z): 620-700 amu. Results Stachyose had a good linear relationship between peak area and concentration in the range of 80-120 μg / ml (r = 0.9992), and the relative standard deviation (RSD) was 0.73%. The recoveries of all the three addition levels were 93.0 % ~ 105.8%. Conclusion The method is rapid, selective and specific, analysis time is short and no derivatization, anti-interference ability, accurate and rapid determination of stachyose content.