本文選題：氫氯噻嗪 + 利尿劑　； 參考：《藥物分析雜志》2017年05期

【摘要】：目的:開發(fā)微量甲醛和甲酸在原料藥中的測定方法。方法:本文建立了一種新型便捷的測定氫氯噻嗪原料藥中殘留甲醛和甲酸的乙醇衍生頂空氣相色譜分析方法,并對建立的方法進行分析方法學(xué)驗證。在本文檢測條件下,甲醛被衍生化成二乙氧基甲烷,甲酸被衍生化成甲酸甲酯。結(jié)果:甲醛的最低檢測限為31μg·g~(-1),最低定量限為100μg·g~(-1),甲醛的回收率在90.0%~110.0%之間,甲醛和二乙氧基甲烷之間的轉(zhuǎn)化率為99.7%;甲酸的最低檢測限為30μg·g~(-1),最低定量限為99μg·g~(-1),甲酸的回收率在90.0%~110.0%之間,甲酸和甲酸乙酯之間的轉(zhuǎn)化率為100.5%。氫氯噻嗪原料藥在該色譜條件下不干擾測定,使用建立的方法對不同批次的氫氯噻嗪進行檢測,均未檢出甲酸,甲醛含量在最低定量限水平以下。結(jié)論:本方法經(jīng)方法學(xué)驗證,適用于氫氯噻嗪原料藥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.
【作者單位】： 浙江大學(xué)藥學(xué)院;浙江華海藥業(yè)股份有限公司;
【分類號】：O657.71;R927.2

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