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
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摘要: 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40 min,用CP-WAX毛细管色谱柱(30 m×0.25 mm,0.25 μm)分离,氢火焰离子化检测器检测.丙酮的质量浓度在0.05~120 mg·L-1范围内与其峰面积呈线性关系,检出限(3S/N)为0.015 mg·L-1.乙醇的质量浓度在0.25~120 mg·L-1范围内与其峰面积呈线性关系,检出限(3S/N)为0.25 mg·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%.Abstract: 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,0.25 μm) 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.
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