冠心苏合丸气相色谱定量指纹图谱研究

Gas chromatography quantified fingerprints of Guanxin Suhe pills

目的建立冠心苏合丸（Guanxin Suhe pill,GXSHP）气相色谱定量指纹图谱质量控制方法。方法采用GC法,FF AP毛细管柱（30 m×0.2 mm,0.33μm）;柱温：程序升温,初始温度70℃,保持1 min,以8℃·min-1升至22 0℃,保持10 min,以1℃·min-1升至245℃;进样口温度260℃,检测器温度280℃,进样量为1μL,分流比为10：1。根据GXSHP-GC指纹图谱特征,用系统指纹定量法鉴定12批次GXSHP质量,并对部分样品质量等级低的原因进行了有效分析。结果以苯甲酸苄酯为参照物峰,确定22个共有指纹峰,建立了GXS HP-GC定量指纹图谱。用系统指纹定量法鉴别出S8质量很好,S1~S7、S9质量好,S12质量一般,S10、S11质量为劣,造成S10、S11的质量等级低的原因是样品中冰片含量高。冰片双组分含量相似度Pm（BN）与全指纹峰整体定量相似度Pm相关系数为0.997 5,冰片中龙脑与异龙脑含量比的均值为1.46（RSD=3.1%）,但龙脑和异龙脑总量波动较大,因此是生产控制重点。不含冰片的多个非极性组分指纹含量约为6.46%（RSD=3.0%）。结论所建立的GXSHP-GC定量指纹图谱可有效反映各批次GXSHP非极性组分总量差异,为GXSHP质量控制提供了新思路和新方法。

Objective To develop gas ch romatography（GC） quantified fingerprints（FP） of Guanxin Suhe pill（GXSHP） to evaluate its quality.Methods GC was perfor med on FFAP capillary column（30 m×0.2 mm,0.33 μm）.The chromatographic condition was as follows： programmed heating,initial column temperature at 70 ℃ for 1 min,t hen rising to 220 ℃ at 8 ℃·min-1,maintaining 220℃ for 10 min,and then to 245℃ at 1℃·min-1.The injector temperature was 260 ℃,the detector temperature was 280℃,the injection volume was 1 μL,and the ratio of splitting was 10∶1.Sys tematically quantified fingerprint method（SQFM） was applied to evaluate the GXSHP-GC fingerprints and identify the quality of GXSHP,and the reason for the low quality grade of some samples was determined.Results GC was used to establish the quantified GC fingerprints and 22 co-possessing peaks were m arked by choosing benzyl benzoate（BB） peak as the reference peak.The quality of S8 was very good,that of S1-S7 and S9 was good,that of S12 was common and that of S10 and S11 was inferior.The reason for the low quality grade of S10-S11 was the high content of borneol in the sampl es.The correlation coefficient between bicomponent of t he micro quanti tative similarity Pm（BN）and the micro quantitative similarity Pm for overall fingerprint was 0.9975.The mea n of content ratio for borneo l to isoborneol was 1.46（RSD = 3.1%）,the total quantity of borneol and isoborneol fluctuated heavily,so both of them shou ld be the key points in the process control.The contents of multiple nonpolar componen ts without borneol were about 6.46%（RSD = 3.0%）.Conclusion This method can clearly and quantitatively disclose the differences among batches and provide a novel method for the quality control of GXSHP.