GC-MS法测定艾拉莫德中磺酸酯杂质

Determination of methanesulfonates impurities in Iguratimod by GC-MS

目的建立气相色谱质谱方法测定艾拉莫德中甲磺酸甲酯(MMS)、甲磺酸乙酯(EMS)、甲磺酸异丙酯(IMS)的含量。方法采用柱前衍生化,将甲磺酸甲酯(MMS)、甲磺酸乙酯(EMS)、甲磺酸异丙酯(IMS)分别衍生成碘甲烷、碘乙烷和碘代异丙烷,采用GC-MS法进行测定。结果 MMS、EMS、IMS分别在8.10×10^(-2)^(-1).53、4.89×10^(-2)^(-1).55、1.02×10^(-1)^(-1).51 mg·L^(-1)内,线性关系良好(r>0.99);MMS、EMS、IMS检测限分别为1.62×10^(-2)、7.30×10^(-3)、2.29×10^(-2) mg·L^(-1),定量限分别为8.10×10^(-2)、4.89×10^(-2)、1.02×10^(-1) mg·L^(-1);在50%、100%、150%水平回收率均在80%~120%内。结论该方法准确可靠,灵敏度高,可用于测定艾拉莫德中甲磺酸甲酯、甲磺酸乙酯、甲磺酸异丙酯的含量。

Objective To establish a method for determination of methyl methanesulfonate(MMS), ethyl methanesulfonate(EMS) and isopropyl methanesulfonate(IMS) in Iguratimod by GC-MS.Methods Method The methyl methanesulfonate(MMS), ethyl methanesulfonate(EMS) and isopropyl methanesulfonate(IMS) were derived into methyl iodide, ethyl iodide and isopropyl iodide by Pre-column derivatisation, respectively, and determined by GC-MS.Results The calibration curves for MMS,EMS and IMS were good linear in the range of 8.10×10^(-2)^(-1).53,4.89×10^(-2)^(-1).55,1.02×10^(-1)^(-1).51 μg·mL^(-1), respectively(r>0.99).The limit of detection of MMS, EMS and IMS were 1.62×10^(-2),7.30×10^(-3) and 2.29×10^(-2) μg·mL^(-1), respectively, the limit of quantitation were 8.10×10^(-2), 4.89×10^(-2),1.02×10^(-1) μg·mL^(-1),respectively;the recoveries at 50%,100%,150% levels were between 80% and 120%.Conclusion The method is accurate, reliable and sensitive, and it′s suitable for the determination of methyl methanesulfonate, ethyl methanesulfonate and isopropyl methanesulfonate in Iguratimod.