毛细管气相色谱法测定盐酸吉西他滨中有机溶剂残留量

Determination of Residual Organic Solvents in Gemcitabine Hydrochloride by Capillary GC

目的建立测定盐酸吉西他滨中有机溶剂残留量的毛细管气相色谱法。方法使用配置顶空进样的气相色谱仪,用DB-624型毛细管色谱柱(94%二甲基聚硅氧烷和6%氰丙基硅氧烷),柱温为40℃,保持5 min,以10℃/min的速度升温至80℃,保持3 min;以氮气为载气,流速25 cm/min;以氢火焰离子化检测器,建立盐酸吉西他滨中甲醇、丙酮、异丙醇、乙酸乙酯的测定方法。结果甲醇、丙酮、异丙醇、乙酸乙酯的质量浓度分别在0.000 3～0.006μg/mL,0.000 5～0.01μg/mL,0.000 5～0.01μg/mL,0.000 5～0.1μg/mL范围内与相应的峰面积呈良好的线性关系,r分别为0.996 6,0.998 7,0.998 6,0.999 7,平均回收率分别为93.53%,107.57%,97.03%,99.63%,RSD均小于5%,检测限分别为2.0×10-6,3.3×10-6,1.4×10-6,4.9×10-8 mg/mL。3批样品中丙酮含量分别为0.04%,0.04%,0.07%,其他溶剂均未检出。结论该方法简单方便、灵敏度高、重复性好、结果准确,适用于盐酸吉西他滨中多种有机溶剂残留量的测定与控制。

Objective To establish a capillary gas chromatography（CGC） method for the determination of four residual organic solvents in gemcitabine.Methods The CGC method was quipped with a headspace injector and a flame-ionization detector.The DB-624 capillary chromatographic column（coated with 94% dimethyl polysiloxane and 6% cyanopropyl-polysiloxane stationary phase） was adopted and the carrier gas was nitrogen.The flow rate was 25 cm/min.The initial column temperature was kept at 40 ℃ for 5 min,then raised to 80 ℃ at the rate of 10 ℃/min and kept at 80 ℃ for 3 min.Results The determination method of methanol,acetone,isopropanol and ethylacetate in gemcitabine was established by hydrogen flame ionization detector（HFID）.Conclusion This method is reliable with high precision,accuracy,specificity,detectability,linearity and durability.It is applicable to the detection of residual organic solvents in gemc-itabine.