加味四物汤GC指纹图谱及含量测定  

Determination of GC fingerprints of flavored Siwu Decoction

作　　者：刘骄楠 赵雨歆 赵旻[1] 谢晓玉 赵春杰[1] LIU Jiaonan;ZHAO Yuxin;ZHAO Min;XIE Xiaoyu;ZHAO Chunjie(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China;Dalian Jinpu New Area Market Supervision and Regulation Service Center,Dalian 116100,China)

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016 [2]大连金普新区市场监管事务服务中心,辽宁大连116100

出　　处：《沈阳药科大学学报》2024年第12期1616-1626,共11页Journal of Shenyang Pharmaceutical University

基　　金：沈阳药科大学2021年度大学生创新创业训练计划项目(202110163025)。

摘　　要：目的建立中药复方制剂四物汤的GC指纹图谱检测方法,同时应用内标曲线法对其中7种挥发性成分进行含量测定。方法采用DB-5毛细管色谱柱(30 m×0.32 mm,0.5μm),程序升温,检测器为氢火焰离子检测器(FID),检测器温度为270℃,气化室温度为250℃,载气为高纯氮气,流量为1.0 mL·min^(-1),分流比为10:1,以α-蒎烯为参比峰,对其进行方法学验证,建立10批药材的GC指纹图谱,采用中药色谱指纹图谱相似度评价软件(2012年版)进行相似度评价;并以β-石竹烯为内标,采用内标曲线法同时测定药品中7种成分的含量。结果建立了10批药材挥发油的GC指纹图谱,各成分的相似度在0.941~0.996之间,共标定出31个共有峰,并指认出其中7个色谱峰;定量分析条件方法学考察结果良好,10批药品中α-蒎烯、桉油精、萜品油烯、樟脑、龙脑、4-萜烯醇、棕榈酸的平均含量分别为0.0067、0.0184、0.0026、0.0013、0.0015、0.0123、0.0259 mg·g^(-1)。结论建立的加味四物汤GC指纹图谱及7种挥发性成分的含量测定方法,精密度、重复性和稳定性均符合要求,可为四物汤的质量控制提供参考。Objective To establish a GC fingerprint detection method for Siwu Decoction,and determine the contents of seven volatile components by internal standard curve method.Methods The DB-5 capillary column(30 m×0.32 mm,0.5μm)was used,the detector was FID,the detector temperature was 270℃,the gasification chamber temperature was 250℃,the carrier gas was nitrogen,the flow rate was 1.0 mL·min^(-1),and the split ratio was 10∶1.Usingα-pinene as reference peaks,methodological verification was carried out to establish GC fingerprints of 10 batches of Chinese medicinal materials,and similarity evaluation software(2012 edition)was used to evaluate the similarity of chromatographic fingerprints of Chinese medicinal materials.Usingβ-caryophyllene as internal standard,the contents of 7 components were determined simultaneously by internal standard curve method.Results GC fingerprints of 10 batches of volatile oil were established,and the similarity of each component ranged from 0.941 to 0.996.A total of 31 common peaks were identified,and 7 chromatographic peaks were identified.The results of quantitative analysis and conditional methodology were good.The average contents ofα-pinene,cineole,terpinolene,camphor,borneol,4-terpineol and palmitic acid in the 10 batches were 0.0067,0.0184,0.0026,0.0013,0.0015,0.0123 and 0.0259 mg·g^(-1).Conclusion The established GC fingerprint of flavored Siwu Decoction and the method for the determination of 7 volatile components met the requirements of precision,repeatability and stability,which can provide a reference for the quality control of Siwu Decoction.

关 键 词：四物汤 GC指纹图谱 质量控制 含量测定 

分 类 号：R917[医药卫生—药物分析学]