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

    • 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–1r≥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.

       

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