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目的:建立气相色谱法测定乌洛托品原料药中甲醛的含量。方法:采用毛细管气相色谱法测定,色谱柱为HP-5石英毛细管柱(30m×0.32mm×0.25μm),程序升温,初始温度为60℃,持续时间4min,以100℃.min-1升温至200℃,保持9min。FID检测器,内标法定量。结果:在确定的色谱条件下,甲醛浓度在21.12～845.80μg·mL-1范围内,线性关系良好,加样回收率为97.7%～101.3%,最低检出限为2.26ng。该方法灵敏度和准确度均符合要求,方法可靠,可用于乌洛托品中甲醛含量的测定。
Objective: To establish a method for the determination of formaldehyde in urotropin raw materials by gas chromatography. Methods: The capillary column was HP-5 quartz capillary column (30m × 0.32mm × 0.25μm). The temperature was programmed at 60 ℃ for 4min and the temperature was raised to 100 ℃ .min-1 200 ℃, hold 9min. FID detector, internal standard method. The results showed that the linearity of formaldehyde concentration was within the range of 21.12-845.80μg · mL-1, the recoveries were 97.7% -101.3% and the minimum detectable limit was 2.26ng under the determined chromatographic conditions. The sensitivity and accuracy of the method are in line with the requirements, the method is reliable, can be used for the determination of urotropine formaldehyde content.