气相色谱-质谱法检测川芎定痛胶囊的挥发油成分

Determination of Components in Volatile Oil from Chuanxiong Dingtong Capsules by the GC-MS

目的建立检测川芎定痛胶囊中挥发油成分的气相色谱-质谱(GC-MS)法。方法采用水蒸气蒸馏法提取样品中的挥发油,采用GC-MS法鉴定挥发油中的化学成分。色谱柱为DB-17MS毛细管柱(30 m×0.25 mm,0.25μm),程序升温,进样口温度为240℃,载气为氦(He)气,载气流速为1 mL/min,分流比为20∶1,进样量为1μL;电子轰击离子源,电子能量为70 eV,接口温度为250℃,离子源温度为230℃,四极杆温度为150℃,溶剂延迟6.5 min,采用全扫描监测方式,质荷比扫描范围为60~600。采用面积归一化法计算挥发油化学成分的相对含量。结果分离出49个成分,并确定31个峰对应的化合物。已鉴定的31个峰占流出峰峰面积的86.78%,分离出的成分包括烯类、醇类、酮类、醚类、酚类、酯类、芳香化合物等。结论所建立的方法可用于川芎定痛胶囊中挥发油成分的检测,以及制剂的质量控制。

Objective To establish a gas chromatography-mass spectrometry(GC-MS)method for the determination of the components in the volatile oil from Chuanxiong Dingxiong Capsules.Methods The volatile oil in the sample was extracted by the steam distillation method,and the chemical components in the volatile oil were identified by the GC-MS method.The chromatographic column was DB-17MS capillary column(30 m×0.25 mm,0.25μm),the temperature was programmed,the injection inlet temperature was 240℃,the carrier gas was helium(He),the flow rate of the carrier gas was 1 mL/min,the split ratio was 20∶1,and the injection volume was 1μL.The ionization mode was adopted with electron-bombardment ion source.The electron energy was 70 eV,the interface temperature was 250℃,the ion source temperature was 230℃,the quadrupole rod temperature was 150℃,and the solvent delay time was 6.5 min.The full-scanning monitoring mode was adopted,and the scanning range of mass-to-charge ratio was 60-600.The relative contents of chemical components in volatile oil were calculated by the area normalization method.Results A total of 49 kinds of components were isolated,and the compounds corresponding to 31 peaks were identified.The identified 31 peaks area accounted for 86.78%of the outflow peak area,and the separated components included alkenes,alcohols,ketones,ethers,phenols,esters and aromatic compounds.Conclusion The established method can be used for the determination of components in volatile oil from Chuanxiong Dingtong Capsules and the quality control of preparations.