GC-MS/MS测定宽胸气雾剂中12种指标成分

目的: 建立气相色谱-三重四极杆质谱(GC-MS/MS)同时测定宽胸气雾剂中桉油精、龙脑、甲基丁香酚、异龙脑、α-红没药醇、榄香素、反式橙花叔醇、石竹烯、α-葎草烯、β-蒎稀、α-蒎稀、左旋樟脑等12种指标性成分方法。方法: 采用内标法,样品经乙醇稀释,GC-MS/MS测定,程序升温,MRM模式检测;并使用热图聚类和主成分分析法对数据进行统计分析。结果: 12种指标成分分别在1~10 ng·mL^-1和50~1 000 ng·mL^-1两个量级内呈线性;回收率为97.5%~104.8%,RSD为1.14%~2.89%(n=3);8批样品中上述成分含量分别为22.24~26.79,22.22~26.88,20.74~22.99,13.72~16.78,10.25~11.23,5.25~5.81,4.60~4.78,2.63~3.06,2.18~2.47,1.92~2.18,1.55~1.94,1.02~1.07 mg·mL^-1;热图聚类分析结果表明同一企业不同批次样品整体质量一致性较好。结论: 该方法专属性强、灵敏度高、测定方法简便结果准确,可为宽胸气雾剂的质量控制提供检验依据。

Determination of 12 index components in Kuanxiong Aerosol by GC-MS/MS

OBJECTIVE To establish a gas chromatography triple tandem quadrupole mass spectrometer (GC-MS/MS) method for the determination of 12 indicative components in Kuanxiong Aerosol,including eucalyptol,borneol,methyleugenol,isoborneol,α-bisabolol,elemicin,nerolidol,caryophyllene,α-humonene,β-pinene,α-pinene,L-camphor.METHODS The samples were diluted by ethanol,determined by GC-MS/MS,temperature programmed,and detected by MRM mode.The data were statistically analyzed by heat map clustering and principal component analysis.RESULTS The 12 index components showed linearity in the scale of 1-10 ng·mL^-1 and 50-1 000 ng·mL^-1,respectively.The recovery rate was 97.5% to 104.8%,and the RSD was 1.14% to 2.89%(n=3).The contents of 12 components in 8 batchs of samples were 22.24-26.79,22.22-26.88,20.74-22.99,13.72-16.78,10.25-11.23,5.25-5.81,4.60-4.78,2.63-3.06,2.18-2.47,1.92-2.18,1.55-1.94,1.02-1.07 mg·mL^-1,respectively.The heat map cluster analysis showed that the overall quality consistency of different batches of samples from the same enterprise was good.CONCLUSION This method has strong specificity,high sensitivity,simple determination method and accurate results,which can provide a test basis for the quality control of Kuanxiong Aerosol.