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[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)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)11.21 mg/L,定量检测限(LOQ)218.7 mg/L,线性相关系数0.999 6,回收率为97.20%~113.0%,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、4.48 mg/L,定量检测限(LOQ)分别为370.9、169.5、438.7、215.7 mg/L,线性相关系数分别为0.9991、0.9998、0.9997、0.9996,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。
[Objective] The study was designed to simultaneously detect the components of respiratory system irritation (light solvent oil) and the chronic toxicity component (xylene) in pesticide cream formulations by capillary gas chromatography. [Method] Non-polar capillary column was used to complete the combination of m / p xylene 2 components into one single peak, which obviously improved the tailing of each peak. Secondly, the column temperature In the detection of the use of “isocratic column temperature ” rather than the traditional “gradient temperature” mode; choose a unique internal standard. The above are conducive to the detection of multicomponent formulations of mutual interference and quantitative accuracy. [Result] The detection limit (LOD) of metaxylene was 11.21 mg / L, the limit of quantification was 218.7 mg / L, the linear correlation coefficient was 0.999 6, the recovery was 97.20% ~ 113.0%, the detection accuracy RSD was 0.207% ~ 2.467% respectively. The LODs of benzene, toluene, m-xylene and orthoxylene were 4.588, 4.044, 8.952 and 4.48 mg / L, respectively. The LOQs were 370.9, 169.5 and 438.7 , 215.7 mg / L respectively. The linear correlation coefficients were 0.9991,0.9998,0.9997,0.9996 respectively. The recoveries were 90.67% -113.2%. The detection accuracy RSD was 0.121% -4.628%. [Conclusion] The method is simple, practical, low cost and suitable for quality control and market regulation.