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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。
Objective: To develop a method for the determination of trace formaldehyde and formic acid in bulk drugs. Methods: A new and convenient method for the determination of residual formaldehyde and formic acid in raw materials of hydrochlorothiazide by headspace gas chromatography was established. The established method was validated by analytical method. For the purposes of this study, formaldehyde was derivatized to diethoxymethane and formic acid was derivatized to formic acid methyl ester. Results: The detection limit of formaldehyde was 31 μg · g -1, the lowest limit of quantification was 100 μg · g -1, the recovery of formaldehyde was between 90.0% and 110.0%, the formaldehyde and diethoxymethane With the lowest detection limit of 30μg · g -1, the lowest limit of quantification was 99μg · g -1, the recovery of formic acid was between 90.0% and 110.0% The conversion between formic acid and ethyl formate was 100.5%. Hydrochlorothiazide API does not interfere with the determination of the chromatographic conditions, the use of established methods for the detection of different batches of hydrochlorothiazide, were not detected formic acid, formaldehyde content below the lowest limit of quantification. Conclusion: This method is validated by methodology and is applicable to the control of trace formaldehyde and formic acid in hydrochlorothiazide bulk drugs.