UPLC-MS/MS法同时测定火炬树茎枝中没食子酸等7种化学成分的含量

Simultaneous determination of seven chemical constituents in Rhus typhina L. stem by UPLC-MS/MS

目的建立同时测定火炬树茎枝中没食子酸、1-O-没食子酰基-β-D-葡萄糖、没食子酸甲酯、黄颜木素、芦丁、槲皮素和1,2,3,4,6-五-O-没食子酰基-β-D-葡萄糖含量的UPLCMS/MS方法。方法采用色谱柱为Thermo Hypersil GOLD C18（50 mm×2.1 mm,1.9μm）柱,流动相为乙腈（A）-体积分数0.2%甲酸水溶液（B）,梯度洗脱,流速为0.2 m L·min-1,柱温为30℃,选择离子反应监测（SIR）和多反应监测模式（MRM）用于定量测定。结果没食子酸、1-O-没食子酰基-β-D-葡萄糖、没食子酸甲酯、黄颜木素、芦丁、槲皮素和1,2,3,4,6-五-O-没食子酰基-β-D-葡萄糖的分别在质量浓度0.078-2.50、0.135-4.32、0.126-4.03、0.013-0.42、0.013-0.42、0.003-0.10和0.995-31.84 mg·L-1内线性关系良好。7种成分的平均加样回收率为98.6%-102.6%（RSD〈3%,n=6）。结论该方法可为火炬树茎枝的质量控制提供参考依据。

Objective To develop an UPLC-MS/MS method for simultaneous determination of gallic acid, 1 -O-galloyl-β-D-glucose, methyl gallate, fustin, rutin, quercetin and 1,2,3,4,6-penta-O-galloyl-β-D-glucose in Rhus typhina L. stem. Methods Separation was achieved on a Thermo Hypersil GOLD C18 column （50 mm ×2.1 mm, 1.9 μm）with a gradient of acetonotrile and 0.2% formic acid aqueous solution at a flow rate of 0. 20 mL.min1. Quantitation was carried out in selected ion recording mode and multiple reaction monitoring（MRM） mode, and the column temperature was 30℃. Results A calibration curve for gallic acid, 1-O-galloyl-β-D-glucose, methyl gallate, fustin, rutin, quercetin and 1,2,3,4,6-penta-O-galloyl- β-D-glucose,over the range 0. 078 - 2.50,0. 135 - 4.32,0. 126 - 4.03,0. 013 - 0.42,0. 013 - 0. 42, 0. 003 -0. 10 and 0. 995 -31.84 mg·L^-1 was established,respectively. The average recoveries of the seven compounds varied from 98.6% - 102.6% with the relative standard deviation 〈 3%. Conclusions The method is accurate and reliable, and can be used for the quality control of Rhus typhina L. stem.