超高效液相色谱-串联质谱(UPLC-MS/MS)法测定杜仲药材中5个指标成分

Determination of five components in blacks of Eucommia ulmoides by UPLC-MS/MS

目的：建立超高效液相色谱串联质谱法同时测定杜仲药材中的京尼平苷酸、原儿茶酸、绿原酸、松脂醇二葡萄糖苷、松脂醇单葡萄糖苷。方法：采用Waters BEH C18（2.1 mm×100 mm,1.7μm）色谱柱,以0.1%甲酸乙腈溶液-0.1%甲酸水溶液为流动相,梯度洗脱,采用电喷雾电离源（ESI）,以多反应离子监测（MRM）检测。结果：京尼平苷酸、原儿茶酸、绿原酸、松脂醇二葡萄糖苷、松脂醇单葡萄糖苷分别在0.842~68.182,0.040~9.838,0.042~10.101,0.499~121.212,0.378~30.606μg·ml-1范围线性关系良好,平均回收率为93.15%~103.68%,RSD〈3%。精密度、重复性和稳定性良好。结论：本方法能简便有效的定量研究杜仲多种成分,为杜仲药材质量控制提供了新的方法。

ABSTRACt： OBJECTIVE An UPLC-MS/MS method was established for the determination of geniposidic acid, protocatechuie acid,chlorogenic acid,pinoresinol diglucoside and pinoresinol singleglucoside in blacks of Eucommia ulrnoides. METHODS A Water BEH C18 column （2. 1 min× 100 mm, 1.7 μm）was used with the mobile phase of 0.1 % formic acid acetonitrile solution- 0. 1 % formic acid aqueous solution by gradient elution. Multiple reactions monitoring （MRM） mode was used for detection by electro-spray ionization source （ESI）. RESULTS It was linear for geniposidic acid, protocatechuie acid, chlorogenic acid, pi- noresinol diglucoside and pinoresinol singleglucoside in the ranges of 0. 842 - 68. 182,0. 040 - 9. 838,0. 042 - 10. 101,0. 499 - 121. 212 μgoml^-1 and 0. 378 - 30. 606 μgoml^-1 , respectively. The average recoveries were 93. 15%-103. 68%, with RSD less than 3%. Precision, repeatability and stability were good. CONCLUSION The method of measuring components in Eucommia ulmoides is convenient and effective, and can be used for the quality control of Eucommia ulmoides.