超高效液相色谱-串联四极杆飞行时间质谱法定性定量检测硫化胶中促进剂DPG
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摘要
利用超高效液相色谱-串联四极杆飞行时间质谱法,以乙腈+水(含体积分数为0. 000 3的甲酸)为流动相进行梯度洗脱,采用ESI正离子模式,对硫化胶中促进剂DPG进行定性定量分析。结果表明,在质量浓度为1～1 000ng·mL~(-1)范围内,促进剂DPG溶液标准曲线线性关系良好,相关因数为0. 993,检出限为0. 01 ng·mL~(-1),回收率为94. 0%～100. 5%。
A qualitative and quantitative analysis of the accelerator DPG in vulcanizates was established by UPLC/Q-TOF MS,gradient elution with acetonitrile + water(volume fraction of methanoic acid was 0. 000 3) as mobile phase was applied,and ESI source and positive ion mode were used for massspectrometry. The results showed that,the standard curve of accelerator DPG solution had good linearity with the real value in the range of mass concentration from 1 to 1 000 ng·mL~(-1),R~2 was 0. 995,the detection limit was 0. 01 ng·mL~(-1),and the recovery was 94. 0%～100. 5%.
A qualitative and quantitative analysis of the accelerator DPG in vulcanizates was established by UPLC/Q-TOF MS,gradient elution with acetonitrile + water(volume fraction of methanoic acid was 0. 000 3) as mobile phase was applied,and ESI source and positive ion mode were used for massspectrometry. The results showed that,the standard curve of accelerator DPG solution had good linearity with the real value in the range of mass concentration from 1 to 1 000 ng·mL~(-1),R~2 was 0. 995,the detection limit was 0. 01 ng·mL~(-1),and the recovery was 94. 0%～100. 5%.
引文
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[6]HG/T 2342—2010,硫化促进剂DPG[S].
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[2]王作龄,张卓娅.橡胶试验方法(五十)[J].橡塑资源利用,2014(6):43-47.
[3]冉克勤,吕桂中.橡胶促进剂DPG氧气氧化反应的终点测试分析及产品提纯技术[J].橡胶科技,2017,15(4):47-49.
[4]赵世库,王晓东,刘世刚.橡胶硫化促进剂D生产技术现状综述[J].辽宁化工,1999,28(3):21-24.
[5]徐艳林,陈绪飞,高明.高效液相色谱法测定橡胶塑解剂DBD的含量[J].橡胶工业,2018,65(3):344-345.
[6]HG/T 2342—2010,硫化促进剂DPG[S].
[7]荣杰峰,毛树禄,钟坚海,等.超高效液相色谱-串联质谱法测定橡胶产品中4种秋兰姆类硫化促进剂含量[J].分析测试学报,2016,35(4):438-442.