摘要
目的:建立柱前衍生化后HPLC测定聚乙二醇400(PEG400)中甲醛含量的方法。方法:PEG400中加入2,4-DNPH衍生化试剂,在25℃下反应30 min,使用CAPCELL PAK DD-C8柱(4.6 mm×150 mm,5μm)分离,流动相为水-乙腈,梯度洗脱,流速为1.0 m L·min^(-1),检测波长360nm,柱温为30℃。结果:聚乙二醇400中的残留甲醛经衍生化后可实现较好分离测定,甲醛的衍生化效率为90.8%,甲醛-DNPH浓度在0.1~60μg·m L^(-1)范围内有良好的线性关系(r=1),方法平均回收率为90.34%。结论:本方法准确,可靠,重现性好,可作为聚乙二醇400中残留甲醛的质控方法。
To establish an HPLC method for the quantitative determination of formaldehyde in polyethylene glycol 400 （PEG400） with pre-column derivatization. Methods： The derivatization reaction of formaldehyde was carried out at 25℃ for 30min with 2,4-DNPH. The samples were separated on CAPCELL PAK DD-C8 column （4.6mm×150mm, 5μm） by the gradient elution of acetonitrile-water at a flow rate of 1.0ml/min. The detection wavelength was set as 360nm, and the column temperature was set as 30℃. Results： The formaldehyde in PEG400 could be separated and determined by pre-column derivatization. The derivatization efficiency of formaldehyde was 90.8%. There was good linearity in the range of 0.1~60 μg？mL-1 of formaldehyde-DNPH with r=1 and the average recovery as 90.34%. Conclusion： The method is accurate and reliable, and has the good reproducibility.It can be applied to the control of formaldehyde in PEG400.
出处
《中国药品标准》
CAS
2017年第6期465-468,共4页
Drug Standards of China
基金
基金项目:十三五国家新药创制-化药制剂质量关键技术评价研究(2015ZX09303001)
