顶空-气相色谱法测定伊班膦酸钠注射液中丙酮和乙醇残留量

GC Determination of Residual Amounts of Acetone and Ethanol in Sodium Ibandronate Injection with Head Space

采用顶空-气相色谱法测定伊班膦酸钠注射液中丙酮和乙醇的残留量。选择顶空平衡温度和时间分别为70℃和40min,用CP-WAX毛细管色谱柱（30m×0.25mm,0.25μm）分离,氢火焰离子化检测器检测。丙酮的质量浓度在0.05~120mg·L-1范围内与其峰面积呈线性关系,检出限（3S/N）为0.015mg·L-1。乙醇的质量浓度在0.25~120mg·L-1范围内与其峰面积呈线性关系,检出限（3S/N）为0.25mg·L-1。丙酮和乙醇的加标回收率分别在97.0%~112%和94.9%~112%之间。丙酮和乙醇的峰面积相对标准偏差（n=6）分别为2.2%和2.5%。

GC was applied to the determination of residual amounts of acetone and ethanol in sodium ibandronate injection with head space. The equilibrium temperature and time of head space were set at 70℃ and 40 min. The analyte was separated on CP-WAX capillary chromatographic column （30 m×0.25 mm, 0. 25μm） and detected by FID. Linear relationship between values of peak area and mass concentration of acetone was kept in the range of 0. 05-120 mg·L-1 with detection limit （3S/N） of 0. 015 mg· L-1. Linear relationship between values of peak area and mass concentration of ethanol was kept in the range of 0.25-120 mg·L-1 with detection limit （3S/ N） of 0. 25 mg·L-1. Values of recovery found by standard addition method were in the range of 97.0%- 112% for acetone and of 94. 9%-112% for ethanol. Values of RSD＇s （n=6） of peak area found were 2.2% for acetone and 2. 5% for ethanol.