药用复合硬片中甲苯二异氰酸酯单体残留检测

2, 4-TDI Monomer Residue Detection of Drug Composite Sheet

目的检测药品包装材料使用的粘合剂中甲苯二异氰酸酯(2,4-TDI)单体的残留量。方法用乙腈提取样品后,与衍生剂1,2-吡啶哌嗪溶液进行衍生化反应,然后采用反相高效液相色谱法测定衍生物,从而计算2,4-TDI单体残留量,并进行方法学考察。结果衍生物的线性范围为0~1.2μg/mL(线性相关系数R=0.9998,线性拟合点数n=7);精密度的相对标准偏差为1.52%;24 h内稳定性的相对标准偏差为2.51%;回收率平均值为102.63%,回收率的相对标准偏差为1.79%。结论建立的方法可靠、结果准确、稳定性好、专属性强,能够快速测定衍生物的含量,从而计算2,4-TDI单体的残留量,为药品包装材料所使用的粘合剂中2,4-TDI单体残留量的检测提供有力支持。

The work aims to test the 2, 4-TDI monomer residue of the adhesive used in the drug packaging materials. The sample was extracted with acetonitrile and derivatived with 1, 2-pyridyl piperazine. Then, the derived product was tested with RP-HPLC, thus calculating the 2, 4-TDI monomer residue and investigating the methodology. The linear range of derivative was 0~1.2 μg/mL（linearly dependent coefficient R=0.9998, and number of linear fitting points n=7）. The relative standard deviation（RSD） of precision was 1.52% . RSD of stability in 24 h was 2.51% . The mean recovery was 102.63% and the RSD of recovery was 1.79% . The method established is reliable, accurate, stable and specific, and can be used to test the content of derived product rapidly, thus calculating 2, 4-TDI monomer residue, and providing powerful support for the test of 2, 4-TDI monomer residue in the adhesive used by the drug packaging materials.