GC-MS法测定爱维心口服液中麝香酮的含量

Content Determination of Muscone in the Aiweixin Oral Liquid by GC-MS

目的：建立测定爱维心口服液中麝香酮含量的方法。方法：样品经正丁醇萃取后,采用气相色谱-质谱联用法。色谱柱为BD-17MS,进样口温度为270℃,采用程序升温,载气为高纯氦气,流速为1 ml/min,进样量为1μl,分流比为20∶1;采用EI离子源,电子能量为70 e V,离子源温度为230℃,四级杆温度为150℃,调谐方式为自动调谐,质量扫描方式为全扫描,扫描范围为30~600 aum,阈值为30。结果：麝香酮进样量在12.216~61.08 ng范围内与峰面积呈良好的线性关系（r=0.999 6）;精密度试验的RSD〈2%,稳定性、重复性试验的RSD〈3%;平均加样回收率为100.24%,RSD为1.58%（n=6）。结论：该方法灵敏、快速、简单,可用于测定爱维心口服中麝香酮的含量。

OBJECTIVE：To establish the method for the residues determination of 5 organic solvents in teicoplanin raw material and injection. METHODS：Headspace GC was performed on the column with 6% cyanopropylphenyl-94% dimethyl polysiloxane（DB-624）as the stationary phase capillary column,the carrier gas was nitrogen,using the temperature program. The temperature of inlet was 200 ℃,detector was hydrogen flame ionization detector with the flow rate of 1 ml/min,split ratio was 40 ∶ 1 and the volume was 1 ml. RESULTS：Good linearity of ethanol,acetone,ethyl acetate,tetrahydrofuran and triethylamine were obtained（r were 0.999 0-0.999 3）;the average recoveries were respectively 95.6%,97.0%,103.2%,94.3% and 98.2%（RSD were 2.1%-4.9%,n=9）;RSDs of precision and repeatability tests ≤2.6%;and the minimum detectable concentration were respectively 2,2,2,0.7and 0.3 μg/ml. CONCLUSIONS：The established method is rapid,sensitive and accurate,and can be used for the residues determination of organic solvents in teicoplanin raw materials and injection.