建立 ASE-UPLC(快速溶剂萃取仪-超高效液相色谱)法同时测定不同杜仲制剂中京尼平苷酸(GPA)、绿原酸(CA)、松脂醇二葡萄糖苷(PDG)3种指标成分含量的方法.采用70%甲醇水,温度40℃,压力103.4 MPa 的 ASE 法提取;色谱柱 Acquity UPLC BEH C18(100 mm×2.1 mm,1.7μm);乙腈(A)-0.1%甲酸水(B)为流动相;流速0.15 mL/min;洗脱梯度:0~15 min,70%B~90%B;检测波长237 nm;柱温20℃.结果显示3种被测成分分别在选定的范围内线性关系良好;精密度、重复性良好,相对标准偏差(RSD )分别均小于3.0%;平均加标回收率在95.84%~102.69%,RSD 均小于3.0%.表明所建立的方法快捷、准确、重复性好,可用于杜仲制剂中主要成分的含量测定.
An ASE-UPLC method for simultaneous determination of three components including geniposidic acid,chlorogenic acid and pinoresinol diglucoside in the different preparations containing Eucommia ulmoides was established.The ASE extraction was conducted with 70% MeOH-H 2 O as solvent at 40 ℃ and 103.4 MPa, and UPLC analysis was performed on an Acquity UPLC BEH C18 column (100 nm×2.1 mm,1.7 μm)with acetonitrile (A)-0.1% formic acid (B)as mobile phases for gradient elution (0 ~1 5 min,70% B~90% B)at the flow rate of 0.1 5 mL/min.The detection wavelength was 237 nm and the column temperature was 20 ℃. The results showed that three components were separated completely and showed good linearity,precision and repeatability (RSD <3.0% respectively).Recoveries were between 95.84% ~ 102.69% (RSD < 3.0%).The data suggested the established method was rapid,accurate,good reproducible and could be applied to simultane-ously determine main components in the preparations containing Eucommia ulmoides .