摘要
目的:建立六亚甲基二异氰酸酯(HDI)的柱前衍生化反相高效液相色谱法,并用该法测定注射液中HDI的含量。方法:样品经吡啶哌嗪[1-(2-PP)]试液衍生化采用RP-HPLC法测定;色谱柱为Shim-pack VP-ODS(5μm,4.6mm×250mm);流动相:乙腈-水-冰醋酸(62∶38∶0.1,v/v/v;加三乙胺至终浓度为0.005mol·L-1);流速:0.9mL.min-1;柱温:40℃;检测波长:310nm。结果:HDI在浓度为0.03281～0.525μg·mL-1范围内线性关系良好(r=0.9985,n=5),最低检测限为0.02085μg·mL-1。重复测定HDI的RSD为4.70%(n=5),日内及日间精密度分别小于2%和3%,加样回收率为99.11%。结论:本法专属性强、灵敏度高、准确、简便,可用于微量毒性物质HDI的检测。
Objectives：To develop a pre - column derivatization HPLC method for the determination of 1,6 - Hexamethylene diisoeyanate（HDI） from the injection. Methods：The samples were derived with 1 - （2 -Pyridyl）piperazine ,followed by attenuating in acetonitrile. The column for the RP- HPLC was Shim -park VP- ODS（5 μm,4.6 mm ×250 mm） ,and the mobile phase was acetonitrile water - glacial acetic acid（62： 38： 0. 1 ,v/v/v,triethylamine was added to 0. 005 mol·L^-1 at the same time）, with flow rate 0. 9 mL · min^-1 ;the temperature of column was 40 ℃ , and the determination wavelength was set at 310 nm. Results：HDI had a good linearity （r = 0. 9985, n = 5） in the range of 0. 0328 -0. 525 μg·mL^-1 .The RSD of repeated test was 4. 70% （n =5）,and the limit al detection was 0. 0219 μg·mL^-1 . Inter -day RSD was less than 2% and intra -day less than 3% ,respectively. The average recovery of HDI was 99. 11%. Conclusions ： The method was specific, accurate and simple, and can be used for the determination of 1,6 - Hexamethylene diisocyanate.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2009年第7期1159-1162,共4页
Chinese Journal of Pharmaceutical Analysis
