GC-MS/MS测定索法酮中基因毒性杂质异亚丙基丙酮含量

Determination of Genotoxic Impurity Mesityl Oxide in Sofalcone by GC-MS/MS

关键词:  GC-MS/MS  索法酮  异亚丙基丙酮  基因毒性杂质

Key words:  GC-MS/MS  sofalcone  mesityl oxide  genotoxic impurity

摘要:

目的 采用GC-MS/MS测定索法酮中基因毒性杂质异亚丙基丙酮的含量。方法 采用顶空进样法测定，色谱柱为Agilent DB-Heavy WAX （30 m×0.25 mm，0.25 μm），质谱检测器的离子源采用EI源，采集方式为选择性离子监测模式（SIM）。结果 异亚丙基丙酮在0.047 12~1.885 μg·mL^–1（LOQ~200%）内浓度与峰面积线性关系良好（n=6），相关系数（r）为0.999 6，定量限为47.12 ng·mL^–1，检测限为18.85 ng·mL^–1，精密度RSD为1.43%。回收率为84.45%~91.58%，RSD为2.88%，溶液稳定性良好。结论 该方法简便准确，灵敏度高，耐用性好，适用于索法酮中异亚丙基丙酮含量的测定。

Abstract:

OBJECTIVE To establish an headspace sampling coupled with gas chromatography and mass spectrometry method for determination of genotoxic impurity mesityl oxide in sofalcone. METHODS The mesityl oxide in sofalcone was determined by HS-GC-MS with Agilent DB-Heavy WAX(30 m×0.25 mm, 0.25 μm) as stationary liquid capillary chromatographic column. The mass spectrometer was operated in the electron impact ionization(EI) fixed mode. The ion collection mode selected ion monitoring(SIM). RESULTS The linearity of the calibration curve was obtained by according peak area versus concentration of mesityl oxide within 0.047 12-1.885 μg·mL^-1(LOQ-200%) with a regression coefficient(r=0.999 6), which had a good linear relationship. The limit of quantitation(LOQ) was 47.12 ng·mL^-1, the limit of detection was 18.85 ng·mL^-1. The RSD value of the precision was 1.43%. The recoveries with the range of 84.45%-91.58%, the RSD value was 2.88%. The sample solutions were very stability. CONCLUSION The method was convenient, accurate and had high sensitivity, good robustness, which was suitable for determination of mesityl oxide in sofalcone.