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目的:利用离子色谱法建立盐酸阿比朵尔中残留二甲胺的含量测定方法。方法:采用阳离子交换柱[Dionex Ion Pac CG16(5 mm×50 mm)+C S16(5 mm×250 mm)],以30 mmol·L~(-1)甲基磺酸为淋洗液,流速1.0 m L·min~(-1),柱温30℃,电导检测器检测,抑制器为CSRS 300(4 mm)。结果:二甲胺质量浓度在0.031~4.0 mg·L~(-1)范围内线性关系良好(r=0.999 9),二甲胺对照品溶液(1 mg·L~(-1))连续6次进样,保留时间、峰高、峰面积的RSD都小于1.5%,本检测方法的检出限为0.001 mg·L~(-1),定量限为0.004 mg·L~(-1),样品的日内和日间RSD分别为1.7%和2.8%,3个水平的加标提取回收率在94.7%~105.0%之间,3个批次样品中残留二甲胺的含量分别为0.021 2%、0.023 1%、0.020 7%。结论:本方法经方法学验证,可有效监控盐酸阿比朵尔的质量。
OBJECTIVE: To establish a method for the determination of residual dimethylamine in Arbidol hydrochloride by ion chromatography. Methods: Cation exchange column [Dionex Ion Pac CG16 (5 mm × 50 mm) + C S16 (5 mm × 250 mm)] was used with 30 mmol·L -1 methanesulfonic acid as eluent and the flow rate 1.0 m L · min -1, the column temperature was 30 ℃, and the detector was tested with a conductivity detector of CSRS 300 (4 mm). Results: The linear range of dimethylamine was within the range of 0.031-4.0 mg · L -1 (r = 0.999 9), the concentration of dimethylamine was 1 mg · L -1 The RSDs of sub-injection, retention time, peak height and peak area were all less than 1.5%. The detection limit was 0.001 mg · L -1 with the limit of quantification of 0.004 mg · L -1, The RSDs of intra-day and inter-day samples were 1.7% and 2.8% respectively. The recovery rates of spiked samples at three levels were between 94.7% and 105.0%. The contents of residual dimethylamine in three batches were 0.021 2% , 0.023 1%, 0.020 7%. Conclusion: This method is validated by methodology and can effectively monitor the quality of abiraterone hydrochloride.