| 超临界流体色谱—串联质谱分离和测定烟草中磷胺和速灭磷顺反异构体 |
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| 引用本文： | 杨飞,孟红明,崔浩哲,范多青,王颖,刘珊珊,范子彦,唐纲岭,赵蔚.超临界流体色谱—串联质谱分离和测定烟草中磷胺和速灭磷顺反异构体[J].中国烟草学报,2020,26(4):45-55. |
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| 作者姓名： | 杨飞 孟红明 崔浩哲 范多青 王颖 刘珊珊 范子彦 唐纲岭 赵蔚 |
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| 作者单位： | 1.国家烟草质量监督检验中心，郑州高新技术产业开发区翠竹街6号 450001 |
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| 摘 要： | 目的 快速分离和测定烟草中磷胺和速灭磷顺反异构体。 方法 通过超临界流体色谱-串联质谱(SFC-MS/MS)建立了磷胺和速灭磷顺反异构体的分析方法。 结果 结果表明:①磷胺和速灭磷顺反异构体均达到基线分离，分离时间为5 min。②在高、中、低三个不同添加浓度水平下，所有异构体的回收率在84.7%~96.7%之间，日间RSD < 5.0%，检出限(LOD)为0.6 μg/kg~1.7 μg/kg定量限(LOQ)为2.0 μg/kg~5.5 μg/kg。③采用该方法对20个烟叶实际样品进行检测，所有样品均未检出磷胺和速灭磷的异构体。 结论 该方法快速，环保，稳定可靠，可用于分离和测定烟草中磷胺和速灭磷顺反异构体的含量。
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| 关 键 词： | 磷胺 速灭磷 异构体 烟草 串联质谱 超临界流体色谱 |
| 收稿时间： | 2019-10-11 |
Separation and determination of isomers of phosphamidon and mevinphos in tobacco by supercritical fluid chromatography -tandem mass spectrometry |
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| Affiliation: | 1.China National Tobacco Quality Supervision & Test Center, Zhengzhou 450001, China2.Technology Center, China Tobacco Yunnan Industrial Co., Ltd., Kunming 650023, China3.School of Chemistry, Biology and Material Engineering, Suzhou University of Science and Technology, Suzhou 215009, China |
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| Abstract: | To realize rapid separation and determination of isomers of phosphamidon and mevinphos in tobacco, a analysis method of isomers of phosphamine and phosphorous was established by supercritical fluid chromatography-tandem mass spectrometry (SFC-MS/MS). Results showed that: ① The isomers of phosphamidon and mevinphos reached baseline separation and the separation time was only 5 minutes. ② Under optimized conditions, the recoveries for all isomers were within the range of 84.7%-96.7%, with relative standard deviations (RSDs) less than 5.0% at 0.01, 0.05 and 0.2 mg/kg levels. The LOD for all isomers in tobacco varied from 0.6 μg/kg to 1.7 μg/kg and the LOQ varied from 2.0 μg/kg to 5.5 μg/kg. ③ Twenty tobacco samples were tested with this method and no isomers were detected in all samples. The results confirm that the proposed method is environmentally friendly, convenient and reliable for the selective determination of the isomers of phosphamidon and mevinphos in tobacco. |
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