顶空-毛细管柱气相色谱法测定盐酸艾司洛尔中有机溶剂的残留量

Head Space-Capillary Column GC Determination of Residual Amounts of Organic Solvents in Esmolol Hydrochloride

提出了顶空-气相色谱法测定盐酸艾司洛尔中甲醇、乙醇、丙酮、异丙醇、乙醚、吡啶和甲苯7种有机溶剂残留量的方法。选择顶空平衡温度和时间分别为70℃和30min,用DB-1 125-1032毛细管柱分离,火焰离子化检测器检测。7种芳香烃化合物在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.5～3.8mg·L-1之间。在2个浓度水平上做回收试验,加标回收率在96.2%～102.7%之间,相对标准偏差(n=9)在0.69%～3.0%之间。

Head space-GC was applied to the determination of 7 organic solvents, including methanol, ethanol, acetone, isopropanol, diethyl ether, pyridine and methylbenzene, in esmolol hydrochloride. The balanced temperature and time of head space were set out at 70 ℃ and 30 min. The analyte were separated on DB-1 125-1032 capillary column and detected by FID. Linear relationships between values of peak area and mass concentration of 7 organic solvents were kept in definite ranges. Detection limits （3S/N） found were ranged from 0.5 to 3.8 mg .L ^-1. Tests for recovery were performed by addition of mixed standard of 7 organic solvents at 2 concentration levels for 9 parallel determinations, results of recovery found were in the range of 96. 2%-102. 7% with RSD＇s in the range of 0. 69%-3.0%.