GC-MS法同时测定复方牙痛宁搽剂中薄荷脑和冰片的含量

Simultaneous Determination of Menthol and Borneol in Compound Yatongning Liniment by GC-MS

目的:建立GC-MS法同时测定复方牙痛宁搽剂中薄荷脑、冰片含量。方法:色谱柱:SH-Rxi-5Sil MS(30m×0.25mm,0.25μm),分流进样;分流比20∶1,进样口温度300℃,柱箱初始温度70℃,保持2min,以10℃·min;升温至300℃,保持5min,载气:高纯氦气,柱流量1mL/min,进样量1μL。质谱条件:EI离子源,电子能量70eV,离子源温度200℃,接口温度250℃,溶剂延迟时间2min,扫描方式Q3Scan,质量扫描范围:45~500amu,检测器电压0.2kV,选择离子(SIM)模式进行定量,选择m/z95、71分别为冰片(龙脑和异龙脑)和薄荷脑的定量离子。结果:龙脑和异龙脑、薄荷脑的进样质量分别在10.33~1021.90ng(r=0.9999)、11.78~1177.81ng(r=1.0000)和8.04~804.39ng(r=1.0000)范围内线性关系良好;平均回收率分别为100.44%、101.35%和97.92%,RSD分别为2.2%、1.1%和1.2%。结论:该研究建立的方法具有分析速度快、灵敏度高、重复性好的优点,可用于复方牙痛宁搽剂中薄荷脑和冰片的质量控制。

Objective:To develop aquantitative GC-MS method for the simultaneous determination of menthol,borneol and isoborneol in Compound Yatongning liniment.Methods:The SH-Rxi-5Sil MS(30m ×0.25mm,0.25μm)column was used with split injection mode and the ration of 20∶1.The injection temperature was set at 300℃.The initial oven temperature was 70℃,maintained for 2min,then reached to 300℃ with the speed of 10℃ per minutes and maintained for 5minutes.Helium gas was used as carrier gas at the flow rate of 1mL/min and the injection volume was 1μL.Mass spectrometry conditions:EI was chosen as ion source with 70eV,the temperature of ion source was 200℃,interface temperature was 250℃,and the solvent delay time of 2minutes.The scan mode was Q3Scan with mass amu of 45to 500,detector voltage was 0.2kV.The quantitative mode with SIM method and were choose the m/z95,71as the quantification ions for(borneol,isoborneol)and menthol.Results:The good linear range of borneol,isoborneol and menthol were 10.33~1021.90ng(r=0.999 9),11.78~1 177.81ng(r=1.000 0)and 8.04~804.39ng(r=1.000 0),respectively.The average recoveries were 100.44%,101.35%and 97.92%within RSD2.2%,1.1%and 1.2%,respectively.Conclusion:The established method is proved by methodology which has the good advantages of analysis rapidily,high sensitivity and good reproducibility and can be used for the quality evaluation of in Compound Yatongning liniment.