摘要
目的:建立以反相高效液相色谱-质谱法测定益智合剂中痕量成分芍药苷含量的方法。方法:色谱柱为Diamonsil^TM C18反相柱(150mm×4.6mm,5μm),流动相为甲醇-1%甲酸(80:20),流速为0.8mL·min,柱温为25℃;质谱条件为气动辅助电喷雾离子源(ESI),检测方式为负离子多离子反应监测(MRM),用于定量分析的离子对为m/z(525→449)。结果:芍药苷的检测浓度在0.25~10.00mg·L^-1范围内与峰面积积分值呈良好线性关系(r=0.9990);平均加样回收率为100.07%,RSD=4.42%(n=6)。结论:本方法简单、灵敏、结果可靠,可有效控制益智舍剂的质量。
OBJECTIVE : To establish an RP - HPLC - MS method for the determination of Paeoniflorin, the trace constituent in Yizhi mixture. METHODS: The chromatographic separation was performed on DiamonsilTM C18 reversed- phase column (150 mm × 4.6 mm, 5μm) with colunm temperature at 25 ℃ .The mobile phase consisted of methanol- 1% formic acid aqueous solution (80 : 20) at a flow rate of 0.8 mL . min^-1.The MS was performed in negative ESI and muhiple reaction monitoring (MRM) mode with the ion m/ z (525→449) for quantifying. RESULTS: The linear range of Peoniflorin was 0.25-10.00mg . L^-1(r=0.999 0) with the mean recovery of 100.07% (RSD=4.42%, n=6) .CONCLUSION: The method is simple, sensitive and reliable, and can be used for effective quality control of Yizhi mixture.
出处
《中国药房》
CAS
CSCD
北大核心
2008年第3期199-200,共2页
China Pharmacy
基金
广州市中医药卫生科技基金资助项目(2005A035)