气相色谱-质谱同时测定复方薄荷脑滴鼻液中薄荷脑和樟脑含量  

Simultaneous Content Determination of Menthol and Camphor in Compound Menthol Nasal Drops by Gas Chromatography-Mass Spectrometry

作　　者：杨柳[1] 周雅轩[1] 张囡[1] 王雪[2] Yang Liu;Zhou Yaxuan;Zhang Nan;Wang Xue(Tianjin Children’s Hospital,Tianjin 300134,China;Tianjin Medical University,Tianjin 300070,China)

机构地区：[1]天津市儿童医院,天津300134 [2]天津医科大学,天津300070

出　　处：《儿科药学杂志》2023年第11期32-35,共4页Journal of Pediatric Pharmacy

基　　金：天津市教委科研计划项目,编号2020KJ203。

摘　　要：目的:建立院内制剂复方薄荷脑滴鼻液质量评价中含量测定的方法。方法:采用气相色谱-质谱(GC-MS)测定薄荷脑和樟脑含量。GC-MS条件:色谱柱Agilent DB-5MS(30 m×250μm×0.25μm),流速1 mL/min,分流比10∶1,进样口温度300℃,程序升温(90℃保持5 min,以1℃/min升至100℃,保持5 min,以10℃/min升至220℃,保持2 min);质谱离子源:电子轰击(EI)源,温度230℃,四级杆温度150℃,电子能量70 e V,质荷比(m/z)30~800。结果:薄荷脑和樟脑分别在50.20~803.20μg/mL(r=0.9996)和50.10~801.60μg/mL(r=0.9994)浓度范围内与峰面积呈现良好的线性关系,平均回收率101.5%和101.1%,精密度、稳定性、重复性实验结果相对标准偏差(RSD)均<2%。结论:初步建立了复方薄荷脑滴鼻液中薄荷脑和樟脑的含量测定方法,通过GC-MS建立的质量标准准确、重复性好,可用于复方薄荷脑滴鼻液中薄荷脑和樟脑的含量测定和质量控制。Objective:To establish the method for content determination in quality evaluation of compound menthol nasal drops.Methods:Gas chromatography-mass spectrometry(GC-MS)was adopted to determine levels of menthol and camphor.GC-MS conditions included Agilent DB-5MS column(30 m×250μm×0.25μm),flow rate of 1 mL/min,split ratio of 10∶1,injector temperature of 300℃,and temperature program(initial temperature of 90℃ for 5 min,followed by increase of 1℃/min to 100℃ with 5-minute hold,and increase of 10℃/min to 220℃ with 2-minute hold).The mass spectrometer used an electron impact(EI)source with temperature of 230℃,quadrupole temperature of 150℃,electron energy of 70 eV,and mass-to-charge ratio(m/z)range of 30 to 800.Results:Menthol and camphor exhibited excellent linear relationships with peak areas within concentration ranges of 50.20 to 803.20μg/mL(r=0.999,6)and 50.10 to 801.60μg/mL(r=0.999,4),respectively.The average recovery rates were 101.5% and 101.1% for menthol and camphor,respectively.The precision,stability and repeatability experiments yielded relative standard deviations(RSD)of less than 2%.Conclusion:A preliminary quantitative analysis method for menthol and camphor in compound menthol nasal drops has been established.The quality standards developed by using GC-MS are accurate and exhibit good reproducibility,which can be applied for the content determination and quality control of menthol and camphor in compound menthol nasal drops.

关 键 词：复方薄荷脑滴鼻液 薄荷脑 樟脑 气相色谱-质谱 

分 类 号：R917[医药卫生—药物分析学]