摘要
目的建立顶空气相色谱法测定2-氟-2-脱氧-D-葡萄糖(18F-FDG)中乙腈残留量的测定方法。方法采用顶空气相色谱法,色谱柱为聚乙二醇-20000毛细管柱(30 m×0.32 mm×0.5μm),载气为氮气,压力0.3 MPa。火焰电离检测仪(FID)检测器温度为250℃,进样口温度为200℃。顶空进样,平衡温度为80℃,平衡时间30 min,分流比为20∶1。水为溶剂,外标法测定18F-FDG中乙腈的残留量。结果在此色谱条件下,被测物峰面积与检测浓度在所考察范围内具有良好的线性关系,相关系数r=0.999 9。平均回收率102.5%,相对标准误差为2.53%。乙腈的最低检出限为1μg/mL。结论本实验建立的色谱方法灵敏、准确、重复性好,适用于18F-FDG等正电子放射性药物乙腈残留量的检测。
Objective To establish a method for determination of acetonitrile residue in18F-fluorodeoxyglucose(18FFDG) injection by headspace gas chromatography. Methods The acetonitrile residue in18F-FDG injection was separated by PEG-20000 capillary column(30 m×0.32 mm×0.5 μm) with an flame ionization detector(FID). The carried gas was nitrogen. The pressure was 0.3 MPa. The injector temperature and the detector temperature were controlled at 200 ℃ and 250 ℃,respectively. The containers of headspace injector were in equilibrium at 80 ℃ for 30 min. The splitting ratio was 20:1. The sample dissolved in water and external standard method was used. Results Under the chromatographic conditions, the calibration curve of solvent showed a good linear relationship(r=0.999 9) with detected concentration in the experimental range. The average recovery rate was 102.5% with relative standard deviation(RSD) of 2.53%. The detection limit for acetonitrile was 1μg/mL. Conclusion The established method was sensitive, accurate, reproducible and suitable for the determination of acetonitrile residue in18F-FDG injection.
出处
《肿瘤影像学》
2013年第3期245-248,共4页
Oncoradiology
