固相微萃取联用气相色谱测定有机磷农药

Determination of Organophosphorous Pesticides by Solid-phase Microextraction Coupled to Gas Chromatography

以溶胶-凝胶方法制备的聚甲基苯基乙烯基硅氧烷/羟基硅油复合涂层的固相微萃取探头(PMPVS/OH-TSO)联用气相色谱测定了有机磷农药。同时对固相微萃取的最佳条件进行了优化,该探头较商用探头有更高的萃取能力。方法的检测限分别为2.1μg/L(敌敌畏)、1.5μg/L(甲基对硫磷),相对标准偏差均不大于7.4%,线性范围均为2个数量级。对某灌溉水中残留的有机磷农药进行了测定,但以上的OPPs均没有检测到,其回收率分别为83.6%和93.4%。

Solid-phase microextraction （SPME） with a novel fiber coated with polymethylphenylvinylsiloxane（PMPVS） / hydroxy-terminated silicone oil（OH-TSO） by sol-gel approach, coupled to capillary gas chromatography-flame ionization detector （GC-FID）, was used to determine organophosphorous pesticides. Optimization was carried out for the determination of organophosphorous pesticide with SPME fiber. Gompared with commercial available SPME fibers, the sol-gel-coated PMPVS/ OH-TSO had higher extraction efficiency for organophosphorous pesticide. Detection limits of the method for dichlorvos and methyl parathion were 2.1 μg/L, 1.5μg/L, respectively. The relative standard deviation was no more than 7.4 %. The linear ranges for these analytes were over 2 ordcrs of magnitude concentration range. Some water .samples were analyzed, but none of the organophosphorus pesticides was determincd. The recoveries of spiked water samples were 83.6 % and 93.4%, respectively.