乙醇衍生顶空气相色谱测定氢氯噻嗪原料药中微量甲醛和甲酸的含量

发布时间：2018-05-30 10:48

本文选题：氢氯噻嗪 + 利尿剂　；参考：《药物分析杂志》2017年05期

【摘要】：目的:开发微量甲醛和甲酸在原料药中的测定方法。方法:本文建立了一种新型便捷的测定氢氯噻嗪原料药中残留甲醛和甲酸的乙醇衍生顶空气相色谱分析方法,并对建立的方法进行分析方法学验证。在本文检测条件下,甲醛被衍生化成二乙氧基甲烷,甲酸被衍生化成甲酸甲酯。结果:甲醛的最低检测限为31μg·g~(-1),最低定量限为100μg·g~(-1),甲醛的回收率在90.0%~110.0%之间,甲醛和二乙氧基甲烷之间的转化率为99.7%;甲酸的最低检测限为30μg·g~(-1),最低定量限为99μg·g~(-1),甲酸的回收率在90.0%~110.0%之间,甲酸和甲酸乙酯之间的转化率为100.5%。氢氯噻嗪原料药在该色谱条件下不干扰测定,使用建立的方法对不同批次的氢氯噻嗪进行检测,均未检出甲酸,甲醛含量在最低定量限水平以下。结论:本方法经方法学验证,适用于氢氯噻嗪原料药中微量甲醛和甲酸的含量控制。
[Abstract]:Objective: to develop a method for the determination of formaldehyde and formic acid in raw materials. Methods: a new and convenient method for the determination of residual formaldehyde and formic acid in hydrochlorothiazide raw drug by headspace gas chromatography with ethanol derivation was established. In this paper, formaldehyde was derivatized to diethoxymethane and formic acid to methyl formate. Results: the detection limit of formaldehyde was 31 渭 g / g, and the limit of quantification was 100 渭 g / L. The recovery rate of formaldehyde was between 90.0% and 110.0%, and the conversion rate between formaldehyde and diethoxymethane was 99.7%, the detection limit of formic acid was 30 渭 g / g, and the limit of determination was 99 渭 g / L, and the recovery of formic acid was between 90.0% and 110.0%, respectively. The conversion between formic acid and ethyl formate is 100.5%. Hydrochlorothiazide raw materials did not interfere with the determination of hydrochlorothiazide under the chromatographic conditions. The established method was used to detect hydrochlorothiazide in different batches. Formic acid was not detected and formaldehyde content was below the minimum quantitative limit. Conclusion: the method is suitable for the control of trace formaldehyde and formic acid in hydrochlorothiazide crude drug.
【作者单位】：浙江大学药学院;浙江华海药业股份有限公司;
【分类号】：O657.71;R927.2

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