HPLC/ESI-MS法测定巴戟天中的低聚糖

Determination of Oligosaccharides in Morinda officinalis How by HPLC/ESI-MS

采用高效液相色谱-质谱联用技术测定巴戟天中的低聚糖。色谱及质谱条件为:氨基柱Kromasil 100-5NH2,(250×4.6mm),以乙腈-水(70∶30)为流动相,流速0.6mL/min,离子阱质谱检测器,电喷雾电离,负离子模式,扫描范围m/z:300～1200。低聚糖的MS特征离子为:[M-163]-(-单糖基),[M-163-18]-(-单糖基-H2O),[M-1-342]-(-H-二糖)。以外标法测定,低聚糖在0.0095～0.19mg范围内呈线性关系,r=0.9977,检出限为0.1μg,平均加标回收率为97.0%,相对标准偏差为1.16%(n=5)。从10批不同来源的巴戟天药材测定结果发现,低聚糖的含量最高为18.90%,最低为2.72%,同时首次在巴戟天中发现了二聚糖和三聚糖。

This paper determined the oligosaccharides in Morinda officinalis How by HPLC/MS. The measurement conditions were used： Kromasil 100-5NH2, （250 ×4.6 mm） column, acetonitrile-water（70： 30） as mobile phase, at a flow rate of 0.6 mL/min, detected by Trap Mass detection, ESI negative mode, scan range ： m/z 300-1200. The characteristic ions of oligosaccharides are： [ M-163 ] （ -C6 H11 O5 ）, [ M-163-18 ] （ -C6 H 11 O5 -H2 O）, [ M-1-342 ] （ -H-C 12 H22 O11 ）. The calibration curve was liner over a range of 0. 0095-0.19 mg for the oligosaceharides ,r =0.9977 ,the detectable limit is 0.1 μg, the average recovery rate was 97.0%, RSD is 1.16% （n = 5）. From the results of 10 batches, the highest content of oligosaccharides is 18.90%, the lowest content is 2.72%, and discover disaecharide and trisaccharide in Morinda officinalis How at the first time.