目的 建立芪参益气滴丸(QYDP)及其主要挥发性成分降香油的GC指纹图谱,并采用GC-MS对主要共有峰进行指认。方法 采用HP-INNOWax(30 m×0.25 mm,0.25 μm)毛细管柱进行分离。程序升温,初始温度100℃,保持2 min,以3℃/min升至160℃,以1℃/min升至190℃,以5℃/min升至220℃,以10℃/min升至250℃;载气为高纯氮气,体积流量0.5 mL/min;进样口温度230℃,分流比5:1;检测器为FID,检测温度300℃;EI离子源温度230℃,电离电压70 eV,全离子扫描,扫描质量范围m/z 35~600,溶剂延迟8 min。结果 标定了QYDP GC指纹图谱中33个共有峰,降香油GC指纹图谱中25个共有峰,并推测出反式橙花叔醇、氧化橙花叔醇异构体、法尼醇异构体、檀香花烯、降莰烷、β-没药烯、反式-β-檀香醇等23个共有峰成分。各批制剂及降香油指纹图谱相似度均在0.979以上。结论 该方法简单、可靠,可为QYDP及降香油的质量评价与控制提供依据。

Objective To establish the GC fingerprint of Qishen Yiqi Dropping Pills (QYDP) and Dalbergia odorifera oil and identify the common chromatographic peaks by GC-MS. Methods The GC analysis was performed on an Agilent HP-INNOWax capillary gas chromatography column (30 m×0.25 mm, 0.25 μm). The temperature program was as follows:100℃ for 2 min, 160℃ at 3℃/min, 190℃ at 1℃/min, 220℃ at 5℃/min, then 250℃ at 10℃/min; Nitrogen was used as the carrier gas with its flow rate 0.5 mL/min; The sample injection temperature was 250℃ and the split ratio was 5:1; The detector was FID with its temperature of 300℃.MS parameters:MS electron energy of 70 eV, ion source temperature of 230℃, full-ion scan mass range m/z 35-600, solvent delay for 8 min. Results Thirty-three common peaks were found from QYDP and 25 common peaks were found from D. odorifera oil in their GC fingerprints. Twenty-three common peaks in the fingerprint of D. odorifera oil, such as trans-nerolidol,3,7,11-trimethyl- 3,6-epoxy-1,10-dodecadien-7-ol isomers, farnesol isomers, α-santalene, norbornane, and β-bisabolene were identified. The similarity of all batches of QYDP and D. odorifera oil were both over 0.979. Conclusion This method is simple and reliable and can be used to evaluate the quality of QYDP and D. odorifera oil.

国家科技重大专项课题——面向国际的创新中药大平台建设(2013ZX09402202)