LC-MS/MS同时测定灵芝胶囊中7种三萜酸的含量

Simultaneous Determination of Contents of 7 Triterpenoid Acids in Lingzhi Capsule by LC-MS/MS

关键词:  灵芝胶囊  三萜酸  液相色谱-串联质谱法  含量测定  质量控制

Key words:  Lingzhi capsule  triterpenoid acids  LC-MS/MS  content determination  quality control

摘要:

目的 建立同时测定灵芝胶囊中7种三萜酸含量的LC-MS/MS方法。方法 选用Agilent Zorbax SB-C₁₈（3.0 mm×150 mm，0.35 μm）色谱柱，柱温为40℃，进样量5 μL，离子源为电喷雾离子源，负离子模式监测，以氯霉素为内标物，采用多反应监测模式，以乙腈-水（38∶62）为流动相，流速0.3 mL·min^–1。结果 灵芝酸A、B、C₂、F、G、灵芝烯酸D、赤芝酸A的线性范围分别为4.972~497.2，4.927~492.7，4.949~494.9，4.978~497.8，4.990~499.0，5.070~507.0和5.089~508.9 ng·mL^–1（r≥0.999 8），仪器精密度、稳定性和重复性试验的RSD均<5%，加样回收率为98.4%~101.8%，RSD为1.28%~3.71%（n=6）。结论 该方法简单、快速、重复性好，可用于灵芝胶囊中7种三萜酸成分的含量测定，可用于灵芝胶囊质量控制。

Abstract:

OBJECTIVE To establish the LC-MS/MS method for simultaneous determination of contents of 7 triterpenoid acids in Lingzhi capsule. METHODS The determination was performed on Agilent Zorbax SB-C₁₈ column(3.0 mm×150 mm,0.35 μm) with column temperature of 40℃. The injection volume was 5 μL. Ion source was electrospray ion source. Negative ion mode monitoring was conducted and chloramphenicol was used as internal standard. MRM mode was adopted. The acetonitrile-water(38:62) was used as mobile phase with the flow rate of 0.3 mL·min^-1. RESULTS The linear ranges of ganoderic acid A, B, C₂, F, G, ganoderenic acid D and lucidenic acid A were 4.972-497.2, 4.927-492.7, 4.949-494.9, 4.978-497.8, 4.990-499.0, 5.070-507.0, 5.089-508.9 ng·mL^-1(r ≥ 0.999 8), respectively. RSDs of instrument precision, stability and reproducibility tests were all<5%. The recoveries rate were 98.4%-101.8% (RSD=1.28%-3.71%, n=6). CONCLUSION The method is simple, rapid and reproducible, and can be used for content determination of 7 triterpenoid acids in Lingzhi capsule. It can be used for quality control of Lingzhi capsule.