摘要
目的建立一种气相色谱-质谱联用法(GC-MS)同时测定甲磺酸达比加群酯中甲磺酸甲酯、甲磺酸乙酯和甲磺酸异丙酯的方法。方法采用DB-624色谱柱(30 m×0.25 mm,1.4μm);程序升温:起始温度100℃,以15℃·min^(-1)的速率升温至200℃,再以25℃·min^(-1)的速率升温至240℃;进样口温度为220℃,载气为氦气,流速为1.0 mL·min^(-1),进样量为2.0μL。采集模式为选择离子监测(SIM),离子源温度为230℃。通过内标法进行计算。结果3种甲磺酸酯之间的分离度均大于2.0,甲磺酸甲酯、甲磺酸乙酯、甲磺酸异丙酯的线性回归方程分别为Y=0.0130X+0.0524(r=0.9990)、Y=0.0249X+0.0633(r=0.9993)、Y=0.0188X+0.0906(r=0.9985),均在5.0~120.0 ng·mL^(-1)浓度范围内线性关系良好。检出限为1.5 ng·mL^(-1)(0.15 ppm),定量限为5 ng·mL^(-1)(0.5 ppm)。甲磺酸甲酯、甲磺酸乙酯和甲磺酸异丙酯的平均回收率分别为96.28%、97.91%和95.87%,RSD分别为2.83%、2.93%和1.73%。结论本方法简便、快速、准确、专属性强、灵敏度高,适用于甲磺酸达比加群酯中3种甲磺酸酯的检测。
Objective To establish a method for determination of MMS,EMS and IMS in Dabigatran Etexilate Mesylate by GC-MS.Methods The analysis was carried on an DB-624 column(30 m×0.25 mm,1.4μm).The GC oven temperature was programmed with an initial temperature of 100℃,increasing to 200℃by 15℃·min^(-1),then increasing to 240℃by 25℃·min^(-1).The temperature of the injection port and interface was set at 220℃.Helium was used as the carrier gas;the flow rate was 1.0 mL·min^(-1),and the volume of the injection was 2.0μL.Data acquisition was performed with SIM,and the temperature of the ion source was set at 230℃.Calculated by internal standard method.Results The resolutions of the three mathane sulfonates were greater than 2.0.Linear regression equation of MMS,EMS and IMS was Y=0.0130X+0.0524(r=0.9990),Y=0.0249X+0.0633(r=0.9993),and Y=0.0188X+0.0906(r=0.9985).The linearitis of all were good in the range of 5.0~120.0 ng·mL^(-1).The limit of detection was 1.5 ng·mL^(-1)(0.15 ppm),and the limit of quantification was 5 ng·mL^(-1)(0.5 ppm),respectively.The extractive recovery of MMS,EMS and IMS was 96.28%,97.91%and 95.87%,and the RSD was 2.83%,2.93%and 1.73%,respectively(n=9).Conclusion The method was proved to be simple,accurate,rapid,high sensitivity and good selectivity,and suitable for the determination of the three mathane sulfonates in Dabigatran Etexilate Mesylate.
作者
柏建学
柴发永
范锋
BAI Jianxue;CHAI Fayong;FAN Feng(Shandong Center for Food and Drug Evaluation&Inspection,Jinan 250014,China;Cisen Pharmaceutical Co.,Ltd.,Jining 272073,China)
出处
《药学研究》
CAS
2021年第10期652-655,共4页
Journal of Pharmaceutical Research