高效液相色谱串联质谱法测定通心络胶囊中3种化合物的含量

Simultaneous Determination of Three Compounds in Tongxinluo Capsules by UPLC-MS/MS

目的:使用超高效液相色谱串联质谱联用仪(Ultra-high performance liquid chromatography tandem mass spectrometry,UPLC-MS/MS)建立一种能快速检测通心络胶囊中芍药苷、斯皮诺素和人参皂苷Rg1含量的分析方法。方法:采用Agilent Eclipse Plus C_(18)(2.1 mm×50 mm,1.9μm)色谱柱;流动相:0.05%(体积分数)的甲酸水溶液和0.05%(体积分数)的甲酸-乙腈;流速0.3 mL/min,梯度洗脱;柱温40℃;进样量10μL;检测时间8 min。电喷雾离子源(Electrospray ionization,ESI),正/负离子同时扫描,多反应监测(Multiple reaction monitoring,MRM),8 min内能定量分析出通心络胶囊中3种化合物的含量。结果:芍药苷、斯皮诺素和人参皂苷Rg1在线性范围内线性关系良好,相关系数r≥0.998。加标回收率(n=6)分别为:99.93%,114.00%,95.67%,相对标准偏差分别为2.10%,2.15%,4.66%。结论:实验数据表明该分方法简单专一、灵敏度较高、专属性强,可以在8 min内快速检测出通心络胶囊中3种化合物的含量,为通心络胶囊的生产质量控制提供参考。

Objective:To establish an ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method for the simultaneous determination of Paeoniflorin、Spinosin and Ginsenoside Rg1 in Tongxinluon capsules.Method:Agilent Eclipse Plus C_(18)(2.1 mm×50 mm,1.9μm)column was used.The mobile phase was acetonitrile(0.05%formic acid)and water(0.05%formic acid).The flow rate was 0.3 mL/min and the simple volume was 10μL.The column temperature was set 40℃.The methed was used Electro-spray ionization(ESI)with positive/negative ion scanning under Multiple reaction monitoring(MRM)mode.The contents of the three compounds in Tongxinluon capsule can be quantitatively determined within 8 minutes under the established chromatographic conditions.Results:Three components(Paeoniflorin,Spinosin and Ginsenoside Rg1)were found to have good linear relationship within the range of investigation([WT5"BX]r=0.9981;r=0.9996;r=0.9984).The average sample recovery([WT5"BX]n=6)was 99.93%,114.00%,95.67%,and RSDs was 2.10%,2.15%,4.66%.The method was simple,rapid,sensitive and specific for testing three compounds in Tongxinluon capsules.It can be used for the production and quality control of Tongxinluo capsules.