GC-MS法分析利奈唑胺中的两种基因毒性杂质

Determination of acetamide residue in Linezolid by GC-MS

目的采用气相色谱质谱联用法(GC-MS)测定利奈唑胺中的两种基因毒性杂质S-环氧氯丙烷(ECH)与(S)-N-[2-(乙酰氧基-3-氯丙基)]乙酰胺(ACPA)的残留量。方法采用DB-5MS色谱柱(30 m×0.25 mm,0.25μm),柱温采用程序升温,采用单级四级杆质谱检测器,载气以线速度控制模式,初始流量为1.3 mL·min-1,采集模式SIM,不分流进样。结果 ECH、ACPA的线性范围分别为5.119~341.236 ng·mL-1(r=0.9995)、5.308~353.864 ng·mL-1(r=0.9999),平均回收率分别为91.2%、87.5%。结论所用方法操作简便、结果准确、灵敏度及重复性好,可用于利奈唑胺中两种基因毒性杂质的质量控制。

OBJECTIVE To establish a GC-MS method for the determination of the genotoxic impurities of(S)-(+)-epichlorohydrin(ECH) and(S)-N-[2-(Acetyloxy)-3-chloropropyl]acetamide(ACPA) in Linezolid.METHODS DB-5 MS column(30 m×0.25 mm,0.25 μm)and temperature programming were adopted for the determination with MS detector.Carrier gas was helium and the initial flow rate was 1.3 mL·min-1.Acquisition mode was SIM with splitless injection.RESULTS The linear range of ECH was obtained between 5.119-341.236 ng·mL-1(r=0.9995);the linear range of ACPA was obtained between 5.308-353.864 ng·mL-1(r=0.9999).The average recovery of ECH and ACPA were 91.2% and 87.5%,respectively.CONCLUSION The method is simple,accurate,reliable and reproducible.The method can be applied to the genotoxic impurity ECH and ACPA determination in Linezolid.