论文部分内容阅读
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。
Objective: To establish a pre-column derivatization reversed-phase high-performance liquid chromatography (HPLC) of hexamethylene diisocyanate (HDI), and to determine the content of HDI in the injection by this method. Methods: The sample was derivatized with pyridine piperazine [1- (2-PP)] and determined by RP-HPLC. Shim-pack VP-ODS column was used as the mobile phase (5μm, 4.6mm × 250mm) Water-glacial acetic acid (62:38:0.1, v / v / v; addition of triethylamine to a final concentration of 0.005 mol·L-1); flow rate: 0.9 mL.min- : 310nm. Results: The linear range of HDI was 0.03281 ~ 0.525μg · mL-1 (r = 0.9985, n = 5), and the lowest detection limit was 0.02085μg · mL-1. The RSD of repeated determination of HDI was 4.70% (n = 5). The intra-day and inter-day precision was less than 2% and 3%, respectively. The recovery rate was 99.11%. Conclusion: This method is of high specificity, high sensitivity, accurate and simple, and can be used for the detection of trace toxic substances HDI.