大体积进样-气相色谱法测定水中多种痕量有机磷农药

Rapid Determination of 9 Organic Phosphor Pesticide Residue in Water by Gas Chromatography With Large Volume and Temperature-Programmed Injection

建立了大体积进样气相色谱-火焰光度法检测水中多种痕量有机磷农药的方法。重点研究了程序升温汽化（PrV）进样条件的选择，通过对分流排空量、吹扫时间、WV起始温度等PTV参数的选择，优化了测试条件，提高了检测灵敏度。水中9种有机磷农药的线性良好，10ml水样中三乙基偶磷硫酯的检出限为0．01μg／L，硫磷嗪、致螟磷、甲拌磷、乐果、乙拌磷、甲基对硫磷、对硫磷和氨磺磷的检出限可达0．001μg／L。水中添加多种有机磷农药准确度精密度试验，平均回收率为85．8％～108％，相对标准差在3．3％～11．4％之间。与常规方法相比，该方法前处理简单快速、分析成本低，灵敏度、准确度和精密度均符合地表水检测质量的要求，适用于水环境中多种农药残留的快速检测。

A gas chromatographic method for the determination of 9 Organic Phosphor Pesticide Residues in water is described. Large volume injection of samples with a programmed temperature vaporizer （PTV） system is discussed. The PTV injection parameters （Split vent flow, purge time, PTV system temperature） were investigated to find the optimal operating conditions for the analysis. 10ml water sample was extracted with 1.0ml chloroform and then 30μl solvent was injected to GC system. The 9 organic phosphor compounds were separated through EC- 1 capillary column （30m ×0.32 i.d. ×0.25μm） and determined by GC- FPD. Extemal standards were used for quantitative determination. The average recoveries obtained ranged from 85.5 % to 108%. The relative standard deviation were from 3.3% to 11.4% . The detection limits of the method were less than 0.01μg/L. The method is simple, fast, sensitive and accurate for Organic Phosphor Pesticide Residues determination of lots of water samples.