Abstract
Objective To establish a gas chromatography-mass spectrometry(GC-MS)method for identifying the volatile components in Huoxue Xiaotong Tincture and determining the contents of five indicator components.Methods The chromatographic column was the Agilent PEG20M capillary column(30 m×0.32 mm,0.25 μm),the temperature was programmed,the inlet temperature was 230℃,the carrier gas was high-purity helium,the flow rate was 1.0 mL/min,the split ratio was 5∶1(V/V),and the injection volume was 1 μL.The electron impact ion source(component identification)or selective ion monitoring mode(content determination)was adopted,the mass scanning range was m/z 40-500.Results A total of 37 volatile components were identified.The linear ranges of 3-carene,cineole,β-caryophyllene,eugenol and ethyl p-methoxycinnamate were 0.200 2-40.04 μg/mL,0.202 6-40.52 μg/mL,0.299 2-59.84 μg/mL,0.601 0-120.20 μg/mL,0.302 2-60.44 μg/mL(R2>0.999 0,n=7)respectively.The limits of detection(LOD)of the above five components were 3.11,2.94,3.29,7.58,4.35 ng/mL,and their limits of quantification(LOQ)were 10.31,9.75,10.90,25.03,14.49 ng/mL respectively.The RSDsof precision,stability,repeatability tests were all lower than 5%(n=6).The recovery rates of the above five components were 93.01%,91.90%,94.69%,93.42%.92.70%,with RSDs of 4.98%,5.53%,5.04%,4.29%,4.83%,respectively(n=9).Among the 20 batches of samples,the average contents of 3-carene,cineole,β-caryophyllene,eugenol and ethyl p-methoxycinnamate were 1.48,2.07,3.26,8.80,3.59 μg/mL respectively.Conclusion This method is simple,accurate and repeatable,which can be used for the identification and content determination of volatile components in Huoxue Xiaotong Tincture.关键词
活血消痛酊/挥发性成分/气相色谱-质谱联用法/成分鉴定/含量测定Key words
Huoxue Xiaotong Tincture/volatile component/GC-MS/component identification/content determination分类
医药卫生
