毛细管气相色谱法测定伊立替康原料药中的有机溶剂残留

 目的 建立伊立替康中甲醇、丙酮、异丙醇、二氯甲烷和正己烷残留量的毛细管气相色谱测定方法，并用该法测定样品中的有机溶剂残留量。方法 采用毛细管气相色谱法，色谱柱为DM624（6%氰基甲基硅酮）毛细管柱（30 m×530 μm×3.00 μm），载气为氮气，检测器为氢焰离子化检测器，以程序升温方式使甲醇、丙酮、异丙醇、二氯甲烷和正己烷达到完全分离。结果 5种溶剂的线性均良好（r=0.999 7~0.999 9）；平均回收率97.34%~101.2%；RSD 0.28%~8.42%；检测限0.78~3.17 μg/mL。4批样品中的检出的5种有机溶剂残留量均低于中国药典2005版所规定的限度。结论 本文所建立的毛细管气相色谱法快速、准确，适用于伊立替康有机溶剂残留量的测定，有机溶剂残留量均符合中国药典2005版规定。

Determination of residue organic solvents in crude drug of irinotecan by capillary gas chromatography

Objective To establish a capillary gas chromatography (GC) method for determining residual organic solvents in crude drug of irinotecan, and to apply it to determine the residual organic solvents in samples. Methods A simple capillary GC method was established with FID detector. The capillary column was DM624 (30 m×530 μm×3.00 μm). Nitrogen was used as carrier gas. Methanol, acetone, dimethylcarbinol, dichlormethane and n-hexane were separated completely using temperature program. Results A good linearity was obtained in the experimental concentration (r=0.999 7-0.999 9). The recovery was in the range of 97.34%-101.2% with RSD of 0.28%-8.42%. The limit of detection was 0.78-3.17 μg/mL. The content of five residue organic solvents in four batches of samples were lower than the limit of the regulation of Chinese Pharmacopeia. Conclusions The methods are simple, sensitive and accurate. It can be used for the detection of five residual solvents in irinotecan, the residue level of organic solvents is corresponded the regulation of Chinese Pharmacopeia.