HPLC/ESI-MS法测定刺糖中低聚果糖的含量

Determination of Fructooligosaccharide in Alhagi-honey by HPLC/ESI-MS

目的 建立高效液相色谱-电喷雾离子阱质谱法（HPLC/ESI-MS）测定刺糖中低聚果糖含量的方法。方法采用YMC-Pack NH2分析柱（250×4.6 mml.D,S-5μm,12 nm）分离;乙腈-水=70∶30,流速：1.0 m L·min-1。离子阱质谱检测器,电喷雾电离,负离子模式。结果 蔗果三糖的MS特征离子为：[M-161]-（-单糖基）,[M-179]-（-单糖基）,[M-341]-（-二糖）;蔗果三糖在0.013105∽0.20968 mg·m L-1范围线性关系良好,r=0.9992;低、中、高加标回收率分别为96.9%、99.8%、96.7%,相对标准差分别为1.7%、1.7%、1.4%。测定4批刺糖中蔗果三糖的含量,含量最高为13.4%,含量最低为7%。结论 该方法灵敏度高,准确度、精密度良好,可用于刺糖中蔗果三糖的定性及定量分析。

Objective To establish the method for the determination of fructooligosaccharide in Alhagi-honey by HPLC/ESI-MS. Methods The separation was performed on YMC-Paek NH2 Column （250 mm × 4.6 mm, S-5μm, 12 nm）, with acetonitrile-water（70 ： 30） as mobile phase at a flow rate of 1.0 mL ·min-1. The fructooligosaccharide was detected by ion trap mass spectrometric detector with electrospray ionization in ESI negative mode. Results The characteristic ions of kestose GF2 were [M-161]-（-C6H1005）, [M-179]-（-C6H12O6）, and [M-341]-（-ClEH22OII）. The calibration curve was liner in the range of 0.013105-0.20968 mg· mL-1 for kestose （r=0.9992）. The recovery rates of low-, middle-, and high-concentration of kestose were 96.9 %, 99.8 %, and 96.7 %, and RSD was 1.7 %, 1.7 %, and 1.4 % , respectively. The content of kestose from the 4 batches of samples was in the range of 7 %-13.4 %. Conclusion The established method has high sensitivity, accuracy and precision, and can be used for the qualitative and quantitative analysis of kestose from Alhagi-honey.