UPLC-MS快速测定蒙古黄芪中毛蕊异黄酮葡萄糖苷含量方法的建立

Determination of Calycosin 7-O-β-D-Glucopyranoside in Mongolian Milkvetch Root by UPLC-MS

为了促进蒙古黄芪药材质量的快速测定,采用超高效液相色谱-串联三重四极杆质谱法(UPLC-MS)对不同产地当年移栽蒙古黄芪中毛蕊异黄酮葡萄糖苷的含量进行测定。利用超声法辅助甲醇法提取目标产物,Thenmo-C18(Hypersil GOLDaO,100 mm×2.1 mm,1.9μm)色谱柱检测,在多反应监测(MRM)模式下,以447/142.98 m/z和447/284.64 m/z为定性离子对,447/142.98 m/z为定量离子对,用外标法进行定量。结果表明:毛蕊异黄酮葡萄糖苷在0.01875~0.60000μg·mL^(-1)浓度范围内有良好的线性关系(r=0.992),平均加样回收率为96.6%,RSD为2.701%。不同产地药材中毛蕊异黄酮葡萄糖苷含量测定结果显示,通辽市奈曼旗产的含量为0.031%,赤峰市林西县产的含量为0.033%,呼和浩特市产的含量为0.065%,呼和浩特市显著高于通辽市和赤峰市。可见,超声波辅助甲醇UPLC-MS法具有操作简单、灵敏、快捷,结果稳定可靠的特点,适合蒙古黄芪药材中毛蕊异黄酮葡萄糖苷含量的快速测定。

In order to promote the rapid determination of the quality of mongolian milkvetch root the contents of calycosin 7-O-β-D-glucopyranoside in transplanted mongolian milkvetch root from different habitats were determined by Ultra High-Performance Liquid Chromatography tandem triple quadrupole Mass Spectrometry(UPLC-MS).The target product was extracted by methanol method with the aid of ultrasound,and Thenmo-C18(Hypersil Goldao,100 mm×2.1 mm,1.9μm)was detected by HPLC.Under the MRM mode,447/142.98 m/z and 447/284.64 m/z were used as the qualitative ion pairs and 447/142.98 m/z as the quantitative ion pairs,quantitative analysis by external standard method.The results showed that there was a good linear relationship in the concentration range of 0.01875-0.60000μg·mL^(-1)(r=0.992),the average recovery was 96.6%,RSD was 2.701%.The results showed that the content of Tongliao Naiman Banner was 0.031%,Linxi County,Inner Mongolia was 0.033%and Hohhot was 0.065%,respectively,the Hohhot was significantly higher than in Tongliao and Chifeng.The method establisbed in this research is simple,sensitive,rapid and reliable.It is suitable for the determination of calycosin 7-O-β-D-glucopyranoside in mongolian milkvetch root.