摘要
目的:利用气相色谱-质谱联用仪(GC-MS)建立贴敷类医疗器械中樟脑、薄荷脑、冰片的定性和定量分析方法。方法:采用Agilent HP-INNOWax(30 m×0.25 mm,0.25μm)毛细管色谱柱;以氦气为载气,流量为1.0 ml·min^(-1);柱温80℃维持2 min,以10℃·min^(-1)的升温速率升至120℃,维持12 min,再以30℃·min^(-1)的升温速率升至200℃,维持3 min;离子源为电子轰击电离(EI)源,采集模式为全扫描/选择离子检测。结果:能检测出样品中是否添加樟脑、薄荷脑、冰片,并对其进行定量。3种化合物的线性范围分别为1.742～2.177×10~3(r=0.998 9),1.982～2.478×10~3(r=0.998 9),1.999～2.499×10~3μg·ml^(-1)(r=0.999 8),线性关系均良好;平均回收率分别为93.3%,98.8%,94.9%(n=9)。结论:方法简便、灵敏、准确、快速,可用于贴敷类医疗器械中樟脑、薄荷脑、冰片的定性和定量检测。
Objective：To develop a GC-MS method for the determination of camphor,menthol and synthetic borneol in drug-free cataplamat medical devices.Method;The separation was accomplished successfully using an Agilent HP-INNOWax（30 m×0.25 mm,0.25μm） column with temperature programming starting at 80℃,keeping for 2 min,rising to 120℃at a rate of 10℃· min^-1,keeping for 12 min,then rising to 200℃at a rate of 30℃·minmin^-1 and holding for 3 min.Helium was used as the carrier gas at the flow rate of 1.0 ml·minmin^-1.Gas chromatography coupled with EI-MS was established with full scan /selected ion monitoring mode.Result：Camphor,menthol and synthetic borneol could be detected with this method.The linear range of camphor,menthol and synthetic borneol was 1.742-2.177×10^3（r = 0.998 9）,1.982-2.478×10^3（r = 0.998 9） and 1.999-2.499×10^3μg · min^-1（r = 0.9998）,respectively.The average recovery and the relative standard deviation were as follows;93.3%and 2.7%（n=9） for camphor, 98.8%and 7.0%（n =9） for menthol,94.9%and 2.3%（n = 9） for synthetic borneol.Conclusion：The method with accurate and simple property is successfully applied in the assay and quanitative detection of camphor,menthol and synthetic bomeol in drug-free cataplamat medical devices to identify the potential counterfeits.
出处
《中国药师》
CAS
2012年第2期167-169,共3页
China Pharmacist
基金
湖南省科学技术厅科技计划一般项目(编号:2010SK3150)
