毛细管气相色谱法测定紫杉醇原料药中的有机溶剂残留量

Determination of residue organic solvent in paclitaxel in substance by gas chromatography

目的建立紫杉醇原料药中残留溶剂甲醇、丙酮、乙酸乙酯、正庚烷、二氯甲烷、四氢呋喃、正己烷和吡啶的测定方法。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(30m×530μm×3.00μm),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、乙酸乙酯、正庚烷、二氯甲烷、四氢呋喃、正己烷和吡啶达到了完全分离。结果8种溶剂的线性关系、精密度、准确度、灵敏度均达到了预定的分析要求,在紫杉醇原料药中仅检出了正庚烷。结论本法能快速准确的检测8种有机溶剂,可用于紫杉醇原料药质量控制中的有机残留溶剂检查。

Purpose To establish a gas chromatography （GC） method used for determination of residue organic solvent in paclitaxel substance. Methods GC was used for determination of residue organic solvent; column： DM624 capillary column（30 m× 530μm× 3.00μm） ; carrying gas： N2. Methanol, acetone, acetic ether, normal heptane, dichlormethane, tetrahydrofuran, N-hexane and pyridine were separated completely through gradient temperature with flame ionization detector. Results The linearity, precision, accuracy and sensitivity of the eight solvents under condition of this method were complied with the predefined analytical requirements. Ethanol was detected in paclitaxel substance. Conclusions This method （GC） is rapid and accurate to determine the eight solvents as the residue organic solvent in paclitaxel.