张清智,刘雪姣,黄艳军,温劭,吕妍妍.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[J].橡胶科技,2017,15(5):49-52. |
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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 |
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DOI: |
中文关键词: 4,4′-二氨基-3,3′-二氯二苯甲烷 气相色谱-三重四级杆串联质谱 离子对 重现性 |
英文关键词: 4,4′-diamino-3,3′-dichlorodiphenylmethane gas chromatography-triple quadrupole mass spectrometer ion pair reproducibility |
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中图分类号:TQ336;O657.7+1/63 |
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中文摘要: |
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20 eV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0.1 mg·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。 |
英文摘要: |
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 0.1~5.0 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. |
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