建立UPLC—MS/MS同时测定白及药材中的α-异丁基苹果酸(B6)、4-(葡萄糖氧基)-肉桂酸葡萄糖氧基苄酯(B12)、1,4-二[4-(葡萄糖氧)苄基]_2.异丁基苹果酸酯(B14)、1-[4-(葡萄糖氧)苄基]-2-异丁基苹果酸(B17)、二氢菲1(B19)和1,4-二[4-(葡萄糖氧)苄基]-2.异丁基苹果酸酯-2-[4-O-肉桂酰基-6-O-乙酰基]葡萄糖苷(B23)含量的分析方法,采用AcquityUPLCBEHC18柱(2.1mm×50mm,1.7μm);流动相0.1%甲酸乙腈溶液(A)-0.1%甲酸水溶液(B)为流动相,梯度洗脱,采用电喷雾离子源(ESI),多反应离子监测(MRM)模式进行正负离子同步监测。各指标成分之间分离度良好,在选定的浓度范围内线性关系良好(r≥0.9974),平均加样回收率为98.0r7%-103.19%,RSD〈3.04%为,重复性、精密度和稳定性良好。此方法操作简便,快速,灵敏度高,可用于白及药材中主要活性成分的含量测定,并为白及药材的质量控制提供了新方法。
To establish an UPLC-MS/MS method for the simultaneous determination of α-isobutylmalic acid (B6), ble- stroside ( B 12), militarine ( B 14), gymnosides V ( B 17 ), dihydrophenanthrenes 1 ( B 19 ) and gymnosides IX ( B23 ) in Bletilla striata. An Acquity UPLC BEH C18column(2.1 mm×50mm,1.7μm)was used with the mobile phase of 0. 1% formic acid in acetonitrile-0.1% formic acid in water by gradient elution. Multiple reaction monitoring (MRM) mode was used for the detection by electro-spray ionization (ESI) source. The results showed that six components can be well resolved and that in the selected linear range, all calibration curves of the six components showed good linearity ( r ≥ 0.9974). The average recoveries were 98.07 % -103.19%, with RSDs 〈 3.04%. Repeatability, precision and stability were good. The developed method was simple, rapid, sensitive and suitable for the determination of the main active con- stituents in B. Striata. It provided a new method for the quality control of B. Striata.