药用丁基胶塞中硫磺及4,4‘-二辛基二苯胺的HPLC法测定

Determination of Sulphur and 4,4‘-Dioctyldiphenylamine in Butyl Rubber Stoppers for Pharmaceutical Use by HPLC

建立了高效液相色谱法测定药用丁基胶塞中的硫磺和4,4‘-二辛基二苯胺。考察了二者在不同pH值提取介质中的提取量,测定了将其中一胶塞样品应用于重组人胰岛素注射液包装时加速试验中2种添加剂的迁移情况。采用Agilent C_(18)色谱柱,以乙腈∶四氢呋喃∶水(56∶20∶24)为流动相,检测波长285 nm。硫磺及4,4‘-二辛基二苯胺在0.258~103μg/ml浓度范围内线性关系良好,在pH 3.5缓冲液、pH 8.0缓冲液、注射用水及重组人胰岛素注射液中的回收率为87.9%~107.0%,RSD小于5.37%。

An HPLC method was established for the determination of sulphur and 4,4＇-dioctyldiphenylamine in butyl rubber stoppers for pharmaceutical use. The extracted amounts of sulphur and 4,4＇-dioetyldiphenylamine in different extractants with different pH values were determined. The migration behaviors in the accelerated test of two additives in recombinant human insulin injection were investigated as well. It was carried out on an Agilent C18 column with the mobile phase ofacetonitrile ： tetrahydrofuran ： water （56 ： 20 ： 24） at the detection wavelength of 285 nm. It was linear for sulphur and 4,4＇-dioetyldiphenylamine in the range of 0.258-103 -g/ml. Their recoveries were 87.9 %- 107.0 % with RSDs less than 5.37 % in pH 3.5 and pH 8.0 buffer solutions, water for injection and recombinant human insulin injection.