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HPLC-MS/MS法同时测定(炙)淫羊藿配方颗粒中14种成分的含量
Simultaneous content determination of fourteen constituents in (Fried) Yinyanghuo Formula Granules by HPLC-MS/MS
【摘要】 目的 建立高效液相色谱-串联质谱(HPLC-MS/MS)法同时测定(炙)淫羊藿配方颗粒中木兰花碱、2″-O-鼠李糖基淫羊藿次苷Ⅱ、淫羊藿苷、朝藿定B、朝藿定C、奎尼酸、宝藿苷Ⅰ、箭藿苷B、箭藿苷A、宝藿苷Ⅱ、隐绿原酸、金丝桃苷、朝藿定A、朝藿定A1的含量。方法 分析采用ZORBAX Eclipse XDB-C18色谱柱(4.6 mm×150 mm, 5μm);流动相乙腈(含0.1%甲酸)-水(含0.1%甲酸),梯度洗脱;体积流量0.8 mL/min;柱温35℃;电喷雾离子源;正负离子扫描;多反应监测模式。再进行主成分分析、正交偏最小二乘判别分析。结果 14种成分在各自范围内线性关系良好(R2≥0.996 1),平均加样回收率90.39%~110.81%,RSD 3.18%~10.71%。执行国家药品标准后,配方颗粒质量较稳定,朝藿定B、箭藿苷B、2″-O-鼠李糖基淫羊藿苷Ⅱ、淫羊藿苷、箭藿苷A、宝藿苷Ⅱ、宝藿苷Ⅰ、朝藿定A、隐绿原酸、金丝桃苷、奎尼酸和木兰花碱是主要差异成分。结论 该方法稳定可靠,可为(炙)淫羊藿配方颗粒质量控制、临床应用、药效物质基础研究提供借鉴。
【Abstract】 AIM To establish an high-performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS) method for the content determination of magnoflorine, 2″-O-rhamnosylicarisideⅡ, icariin, epimedin B, epimedin C, quinic acid, baohuoside I, sagittatoside B, sagittatoside A, baohuosideⅡ, cryptochlorogenic acid, hyperoside, epimedin A and epimedin A1 in(Fried) Yinyanghuo Formula Granules.METHODS The analysis was performed on a 35 ℃ thermostatic ZORBAX Eclipse XDB-C18 column(4.6 mm×150 mm, 5 μm), with the mobile phase comprising of acetonitrile(containg 0.1% formic acid)-water(containg 0.1% formic acid) flowing at 0.8 mL/min in a gradient elution manner, and electron spray ionization source was adopted in positive and negative ion scanning with multiple reaction monitoring mode. Subsequently, principal component analysis and orthogonal partial least squares discriminant analysis were performed.RESULTS Fourteen constituents showed good linear relationships within their own ranges(R2≥0.996 1), whose average recoveries were 90.39%-110.81% with the RSDs of 3.18%-10.71%. After the implementation of national drug standards, the formula granules demonstrated stable quality. Epimedin B, sagittatoside B, 2″-O-rhamnosylicarisideⅡ, icariin, sagittatoside A, baohuosideⅡ, baohuoside I, epimedin A, cryptochlorogenic acid, hyperoside, quinic acid and magnoflorine were taken as main differential components.CONCLUSION This stable and reliable method can provide references for the quality control, clinical application and pharmacodynamic material basis research of(Fried) Yinyanghuo Formula Granules.
【Key words】 (Fried) Yinyanghuo Formula Granules; chemical constituents; content determination; high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS); principal component analysis; orthogonal partial least squares discriminant analysis;
- 【文献出处】 中成药 ,Chinese Traditional Patent Medicine , 编辑部邮箱 ,2026年06期
- 【分类号】O657.63;R286.0
- 【下载频次】51