摘要
以500,50和5μg/mL的甲基膦酸乙酯(EMPA)、甲基膦酸异丙酯(IMPA)、甲基膦酸(MPA)、甲基膦酸频哪酯(PMPA)、硫二甘醇(TDG)为研究对象,以气相色谱-质谱为检测手段,使用正交分析法对衍生时间、衍生温度和衍生试剂用量3个因素之间的交互作用及对衍生效果的影响进行了研究。在所选水平范围内,3个因素不存在交互关系;对于EMPA,IMPA,MPA,PMPA,衍生试剂用量影响>衍生时间影响>衍生温度影响,对于TDG,衍生试剂用量影响>衍生温度影响>衍生时间影响;在3个浓度条件下,衍生温度对于5种化合物的衍生效果没有显著影响;在5μg/mL质量浓度条件下,衍生温度、衍生时间、衍生试剂用量对5种化合物的衍生效果皆没有显著影响。
Ethyl methylphosphonate(EMPA),isopropyl methylphosphonate(IMPA),methylphosphonic acid(MPA),pinacolyl methylphosphonate(PMPA)and thiodiglycol(TDG)at concentrations of 500,50 and 5μg/mL respectively were selected as the research objects.Gas chromatography mass spectrometry was used as the detection method.Orthogonal analysis was used to study the interaction between the derivative time,temperature and dosage of derivative reagent and the influence of the three influencing factors on derivative efficiency.Within the selected horizontal range,there is no interaction between the three influencing factors;for EMPA,IMPA,MPA,and PMPA,the effect results were derivative reagent dosage>derivative time>derivative temperature,for TDG,derivative reagent dosage>derivative temperature>derivative time;under all the three concentrations,the derivative temperature has no significant effect on the derivative of five compounds;at 5μg/mL mass concentration,the derivative temperature,the derivative time,and the amount of derivative reagent had no significant effect on the derivatisation of the five compounds.
作者
邢中方
袁铃
杨旸
吴姬娜
于惠兰
刘石磊
XING Zhongfang;YUAN Ling;YANG Yang;WU Jina;YU Huilan;LIU Shilei(Laboratory of Analytical Chemistry,Research Institute of Chemical Defence,Beijing 102205;State Key Laboratory of NBC Protection for Civilian,Beijing 102205)
出处
《分析试验室》
CAS
CSCD
北大核心
2022年第1期44-49,共6页
Chinese Journal of Analysis Laboratory
基金
国民核生化灾害防护国家重点实验室科研基金项目(SKLNBC2019-12)资助。
关键词
正交
硅烷化衍生
质谱
交互关系
衍生效果
化武相关化合物
orthogonal
silylation derivatisation
mass spectrometry
interaction
derivative effects
chemical-warfare-agent related compounds
