气相色谱法检测农药制剂中呼吸系统刺激组分及慢性毒性组分  

Determination of Respiratory Irritants and Chronic Toxic Components for Pesticide Formulations

作　　者：孙敦伟[1] 刘杨[2] 吴晓红[1] 顾中怡[1] 郭争云[1] 

机构地区：[1]上海出入境检验检疫局,上海200135 [2]上海农药研究所,上海200032

出　　处：《农药》2013年第10期736-739,共4页Agrochemicals

摘　　要：【目的】毛细管气相色谱法同时检测农药乳油制剂中呼吸系统刺激组分（轻质溶剂油1和慢性毒性组分（二甲苯）。[方法]采用非极性毛细管色谱柱，使间／对二甲苯2组分完全合并成1个单峰，明显改善了各峰的拖尾现象；其次，采用了低于现有方法的柱温，在检测段采用了“等度柱温”而不是传统的“梯度程序升温”方式；选用了一个独特的内标物。以上均有利于多组分制剂检测的互扰性和定量的准确性。【结果】偏三甲苯的检测低限（LOD）11．21mg／L，定量检测限（LOQ）218．7mg／L，线性相关系数0．9996，回收率为97．20％-113．O％，检测精度RSD为0．207％～2．467％；苯、甲苯、间／对二甲苯、邻二甲苯的检测低限（LOD）分别为4．588、4．044、8．952、4．48mg／L，定量检测限（LOQ）分别为370．9、169．5、438．7、215．7mg／L，线性相关系数分别为0．9991、O．9998．0．9997、O．9996，回收率为90．67％-113．2％，检测精度RSD为0．121％-4．628％。[结论]该方法简捷、实用、成本低，适用于品质控制和市场规范。[Aims] A capillary gas chromatographic method has been developed for the determination of respiratory irritants（light aromatic solvent naphtha） and chronic toxic components（xylene） for formulants of pesticide emulsifiable concentrate（EC） at the same time. [Methods] It applies non-polar capillary column. It combines the two components of m-,p-xylenes into a single peak and remarkably improves peak tailing. Secondly, it applies the column temperature lower than that in the conventional methods, and uses the ＂isocratic column temperature＂ instead of the ＂gradient column temperature＂ in the testing range. Thirdly, a unique internal standard substance is chosen. All of these are in favor of both interference of testing and accuracy of quantitation for multi-component formulation. [Results] For this method, 1,2,4-trimethylbenzene＇s required limit of detection （LOD） is 11.21 mg/L, limit of quantitation （LOQ） is 218.7 mg/L, the linear correlation coefficient is 0.999 6, the recoveries are 97.20-113.0%, and the RSDs are 0.207-2.467%. Benzene, methylbenzene, m-,p-,o-xylene＇s required limits of detection （LOD） are 4.588, 4.044, 8.952, 4.48 mg/L, limits of quantitation （LOQ） are 370.9, 169.5, 438.7, 215.7 mg/L, the linear correlation coefficients are 0.9991, 0.999 8, 0.9997, 0.999 6, the recoveries are 90.67-113.2%, and the RSD are 0.121-4.628%. [Conclusions] The present method is simple, rapid, practical, and suitable for use in quality control and market supervision.

关 键 词：轻质溶剂油 1 2 4-三甲苯(偏三甲苯) 二甲苯 乳油(EC) 呼吸系统刺激组分 慢性毒性组分 制剂型杂质 

分 类 号：TQ450.7[化学工程—农药化工] O657.71[理学—分析化学]