气相色谱-三重四级杆串联质谱法检测聚氨酯橡胶中4,4′-二氨基-3,3′-二氯二苯甲烷的含量

Determination of Content of 4,4′-Diamino-3,3′-Dichlorodiphenylmethane in Polyurethane Rubber by GC-MS/MS

采用气相色谱-三重四级杆串联质谱(GC-MS/MS)法测定聚氨酯橡胶中的4,4′-二氨基-3,3′-二氯二苯甲烷(MOCA)的含量。结果表明,在碰撞能量为20eV下,以质核比(m/z)为265和229的离子对为定性离子对、m/z为265和195的离子对为定量离子对,将MOCA在(60±5)℃下用丙酮超声提取60 min,用GC-MS/MS对提取液进行测试,MOCA含量在0.1~5.0 mg·L^(-1)范围内,其响应强度与标准溶液浓度的线性关系良好,检出限为0.03 mg·L^(-1),定量限为0.1mg·L^(-1),回收率为90%~110%,相对标准偏差小于6%。本方法测试结果稳定,灵敏度高,重现性好。

The content of 4,4’-diamino-3,3’-dichlorodiphenylmethane（MOCA） in polyurethane rubber was determined by gas chromatography-triple quadrupole mass spectrometry（GC-MS/MS）. MOCA was extracted by acetone under ultrasonication at（60±5） ℃ for 60 min,and the extract was tested by GC-MS/MS. The results showed that the relationship between response intensity and standard solution concentration was linear when the MOCA content was in the range of 0. 15. 0 mg·L-1,the ion pair with mass ratio（m/z）of 265 and 229 was the qualitative ion pair and the ion pair with m/z of 265 and 195 was the quantitative ion pair at the collision energy of 20 eV. The detection limit was 0. 03 mg·L-1,the limit of quantification was 0. 1 mg·L-1,the recovery was 90% 110%,and the relative standard deviation was less than 6%. The method showed the advantages of stable test results,high sensitivity and good reproducibility.