氟化物衍生-固相萃取对甲基膦酸类化合物的GC-MS定性分析检测
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- 英文论文题名：Combination of perfluorinated derivatisation and solid phase extraction(SPE) for the qualitative analyzation of methyl phosphonic acid compound by gas chromatograph-mass spectrometry(GC/MS)
- 论文作者：李晓森 ; 杨旸 ; 吴姬娜 ; 梁龙辉 ; 邢中方 ; 李欣海 ; 刘石磊
- 英文论文作者：Li Xiaosen ; Yang yang ; Wu Jina ; Liang Longhui ; Xing Zhongfang ; Li Xinhai ; Liu Shilei ; State key Laboratory of NBC Protection for Civilian ; Research Institute of Defence
- 年：2016
- 作者机构：国民核生化灾害防护国家重点实验室;
- 论文关键词：化武核查 ; GC-CI/MS ; 衍生 ; 甲基膦酸
- 英文论文关键词：Chemical Weapons Verification ; GC-CI/MS ; Derivatisation ; MPA
- 会议召开时间：2016-07-01
- 会议录名称：中国化学会第30届学术年会摘要集-第三十四分会：公共安全化学
- 语种：中文
- 分类号：O657.63;X832
- 学会代码：ZGHY
- 会议名称：中国化学会第30届学术年会-第三十四分会 ; 公共安全化学
- 会议地点：中国辽宁大连
- 主办单位：中国化学会
- 学会名称：中国化学会
- 页数：1
- 文件大小：258k
- 原文格式：D
- 会议级别：全国
摘要
本文针对水样中的痕量(<1mg/L)甲基膦酸类化合物进行GC-MS的定性分析检测研究。真实样品来源为禁止化学武器组织(OPCW)所组织的第38次水平考试附加的痕量样品。本文针对待测的目标化合物建立了固相萃取结合氟化物衍生的方法进行样品制备。采用600MHz核磁对氟化物衍生前后的标准品进行分析可知,本方法选用的氟化物衍生化效率大于99%。采用气相色谱-电子轰击电离质谱(GC-EI/MS)、气相色谱-化学源负电离质谱(GC-NCI/MS)以及气相色谱-选择离子扫描质谱(GC-SIM-MS)分析方法对五种标准物质沙林(GB)、梭曼(GD)以及甲基膦酸异丙酯(IMPA)、甲基膦酸乙酯(EMPA)以及甲基膦酸(MPA)的衍生化产物进行分析。针对真实样品采用直接进样分析以及氟化物衍生-固相萃取处理后分析,采用气相色谱-选择离子扫描质谱(GC-SIM-MS)分析方法,通过将真实样品的谱图与标准物质谱图对比,最终获得真实样品中痕量添加化合物的信息,添加浓度约为0.2μg/L,检出限低于1ppb。
In our work, the sample was prepared by solid phase extraction(SPE) and perfluorinated derivatisation. The pentafluorobenzoyl derivatisation efficiency reached up to 99% detected by 600 MHz NMR. The GB, GD and the derivatisation product of IMPA, EMPA and MPA were analyzed by Gas chromatography-electron ionization/mass spectrometry(GC-EI/MS) and Gas chromatography-source of chemical ionization/mass spectrometry(GC-NCI/MS). The real sample was measured by Gas chromatography-selection ion scan/mass spectrometry(GC-SIM-MS) after perfluorinated derivatisation. By comparing the spectrograms of standard and real sample, the trace amount of additives was obtained. The detection limit was found less than 1 ppb.
In our work, the sample was prepared by solid phase extraction(SPE) and perfluorinated derivatisation. The pentafluorobenzoyl derivatisation efficiency reached up to 99% detected by 600 MHz NMR. The GB, GD and the derivatisation product of IMPA, EMPA and MPA were analyzed by Gas chromatography-electron ionization/mass spectrometry(GC-EI/MS) and Gas chromatography-source of chemical ionization/mass spectrometry(GC-NCI/MS). The real sample was measured by Gas chromatography-selection ion scan/mass spectrometry(GC-SIM-MS) after perfluorinated derivatisation. By comparing the spectrograms of standard and real sample, the trace amount of additives was obtained. The detection limit was found less than 1 ppb.
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