柱前衍生化HPLC法测定聚乙二醇400中的甲醛  

Determination of Formaldehyde in Polyethylene Glycol 400 by HPLC with precolumn derivatization

作　　者：张朝阳[1] 汤清娟 许凯 晏建磊 杨锐[1] 汤龙[1] 孙会敏[1] 

机构地区：[1]中国食品药品检定研究院,北京100050 [2]运城学院,山西044000

出　　处：《中国药品标准》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)

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.

关 键 词：聚乙二醇400 甲醛 甲醛-DNPH HPLC法 

分 类 号：R921.2[医药卫生—药学]