采用气相色谱法建立氟[^(18)F]脱氧葡糖注射液中有机溶剂残留的测定方法及其方法不确定度的评价

Determination of residual organic solvents in Fluorine[18F] deoxy glucose injection by gas chromatography and evaluation of its uncertainty

目的参考中国药典对氟[^(18)F]脱氧葡糖注射液的质量控制要求,建立对氟[^(18)F]脱氧葡糖注射液中有机溶剂残留的测定方法及其方法不确定度进行评定。方法以SUPELCOSPB-5型毛细管柱作为分离柱,采用气相色谱法对PET示踪剂2-^(18)F-2-脱氧-葡萄糖(^(18)F-FDG)合成制备工艺中所使用的有机溶剂乙腈和乙醇进行定量检测。并对^(18)F-FDG中有机溶剂残留的测定方法的不确定度进行初步评价。结果该药品中两种有机溶剂乙腈及乙醇的残留量在分离柱的保留时间10min;采用此方法随机检测了5批次^(18)F-FDG产品,检测结果显示,^(18)F-FDG中含乙醇0.078g/L,乙腈0.079g/L,均符合2015版《中国药典》中对残留溶剂的限度要求。结论应用气相色谱法对^(18)F-FDG中乙腈和乙醇残留物的快速、定量测定具有良好的重复性,并且分析准确、迅速;对^(18)F-FDG中有机溶剂残留的测定方法的不确定度进行了初步分评价。

Objective To establish a method for the determination of organic solvent residues in fluoro Fluorine[^18F] deoxy glucose injection and to evaluate its uncertainty based on the Chinese Pharmacopoeia quality control requirements of ^18F deoxy glucose injection. Methods A capillary column of SUPELCOSPB-5 was used as the separation column.The organic solvents acetonitrile and ethanol used in the synthesis of PET tracer 2-^18F-2-deoxyglucose（^18F-FDG） were quantitatively detected by gas chromatography.The uncertainty of determination method of residual organic solvents in ^18F-FDG was preliminarily evaluated. Results The residue of the two organic solvents acetonitrile and ethanol in the drug was retained on the separation column for 10 min.5 batch of ^18F-FDG products were randomly detected by this method.The results showed that ^18F-FDG contained ethanol 0.078 g/L and acetonitrile 0.079 g/L,which met the limit requirements for residual solvents in the 2015 edition of the Chinese Pharmacopoeia. Conclusion The rapid and quantitative determination of acetonitrile and ethanol residues in ^18F-FDG by gas chromatography has good repeatability and accurate and rapid analysis.The uncertainty of the determination method of residual organic solvents in ^18F-FDG is preliminarily evaluated.