乌洛托品原料药中甲醛的含量测定

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(30 m×0.32 mm×0.25 μm),程序升温,初始温度为60 ℃,持续时间4 min,以100 ℃·min^-1升温至200 ℃,保持9 min。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21.12~845.80 μg·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2.26 ng。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 GC method for the determination of formaldehyde in urotropine pharmaceutical product. Methods: Capillary gas chromatography(CGC) was adopted with HP-5 silici-capillary column(30 m×0.32 mm×0.25 μm)for the detection,and temperature programming was carried out with 60 ℃ as the initial temperature,lasted for 4 min,then rose to 200 ℃ with the speed of 100 ℃·min^-1,kept for 9 min.FID detector and internal standard method were used for the quantitative analysis. Results: The linear relation of formaldehyde was all right with the concentration in the range of 21.12-845.80 μg·mL^-1under the definite chromatographic condition.The recoveries of spiked samples were ranging from 97.7% to 101.3% and the detection limit was 2.26 ng.Both the sensitivity and accuracy fitted the bill.This method can be successfully used to determine the formaldehyde in urotropine.