顶空气相色谱法测定布美他尼原料药中残留的溶剂

Determination of Residual Solvents in Bumetanide Raw Material by Headspace Gas Chromatography

目的建立测定布美他尼原料药中两种有机溶剂甲苯和乙醇残留量的顶空气相色谱法。方法采用DB-1型石英毛细管柱(30 m×0.53 mm,1.5μm),载气为氮气,FID检测器;程序升温,起始温度35℃维持3 min,再以55℃/min升温至90℃,维持1.5 min。结果两种有机溶剂完全分离,乙醇与甲苯质量浓度分别在3.7～33.3μg/mL(r=0.999 8)及3.6～32.4μg/mL(r=0.999 6)范围内与相应的峰面积之比呈良好的线性关系;平均回收率分别为100.37%和97.01%,RSD分别为0.80%和1.12%(n=9);乙醇、甲苯的最低检测限分别为0.02μg/g和0.05μg/g(S/N=3)。结论该方法灵敏、准确、重现性好,可用于实际生产中的质量控制。

Objective To establish a method for the residual solvent detection of ethyl alcohol and toluene in the raw material of bumetanide by headspace gas chromatography（HS-GC）.Methods The DB-1 capillary column（30 m × 0.53 mm,1.5 μm） with carrier gas of nitrogen and FID test were adopted for the gas chromatography showing.The initial column temperature was kept at 35 ℃ for 3 min,and escalated to 90 ℃ for 1.5 min with the rate of 55 ℃/min.The residual solvents of ethyl alcohol and toluene in bumetanide were determinated.Results Ethyl alcohol and toluene were separated completely and shown as the linear plot within the concentrations of 3.7-33.3 μg /mL（r = 0.999 8） and 3.6-32.4 μg/mL（r = 0.999 6） respectively with a mean recovery rate of 100.37% and 97.01%,RSD was 0.80% and 1.12%,respectively.Their test limitations were 0.02 μg/g and 0.05 μg/g（S/N = 3）.Conclusion This method is sensitive,accurate,repro-ducible,which can be used to the quality control in practical production.