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目的:建立羟尼酮中甲醇、二氯甲烷、N,N-二甲基甲酰胺的残留量的测定方法。方法:采用溶液直接进样法测定羟尼酮中有机溶剂残留量。使用DB-624柱(30m×0.53mm,3μm);以高纯氮气为载气;以FID为检测器。结果:甲醇、二氯甲烷、N,N-二甲基甲酰胺具有良好的线性;精密度的相对标准偏差均小于2%,平均回收率在98.83%～103.70%之间。结论:此方法简单、准确,灵敏度高,可用于羟尼酮中甲醇、二氯甲烷、N,N-二甲基甲酰胺的残留溶剂的测定。
OBJECTIVE: To establish a method for the determination of the residual amount of methanol, dichloromethane and N, N-dimethyl formamide in hydroxyjinone. Methods: Determination of residual organic solvents in hydroxynone by direct injection of solution. A DB-624 column (30 m × 0.53 mm, 3 μm) was used; high purity nitrogen was used as a carrier gas; and FID was used as a detector. Results: Methanol, methylene chloride and N, N-dimethylformamide had good linearity. The relative standard deviations of precision were less than 2% and the average recoveries were between 98.83% and 103.70%. Conclusion: This method is simple, accurate and sensitive. It can be used for the determination of residual solvents of methanol, dichloromethane and N, N-dimethylformamide in hydroxymethyl ketones.