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对水中有机磷农药样品保存方法的优化
引用本文:李钟瑜.对水中有机磷农药样品保存方法的优化[J].环境科学与管理,2013(2):120-123,127.
作者姓名:李钟瑜
作者单位:上海市普陀区环境监测站
摘    要:优化了对水中11种有机磷农药检测的样品保存方法。加标水样在4℃下保存一定时间后,通过液液萃取,气相色谱-质谱(选择离子模式)法测定有机磷农药的回收率。在不加入稳定剂的情况下,水样的保存时间不宜超过16h。为延长样品的保存时间,向水样中加入有机溶剂和pH调节剂作为稳定剂。实验结果表明,当在1000ml样品中加入10ml正己烷和10mlpH=3.6的醋酸-醋酸钠缓冲溶液时,可以将样品保存时间延长至48h。为验证方法的有效性,以地表水作为实际水样,加标浓度水平在0.2μg/L和0.04μg/L时,48h后的平均加标回收率在76.2%-95.0%之间,RSD在2.4%-7.2%之间。

关 键 词:有机磷农药  样品保存  气相色谱-质谱

Optimization of Sample Preservation Method for Organophosphorus Pesticides in Water
Li Zhongyu.Optimization of Sample Preservation Method for Organophosphorus Pesticides in Water[J].Environmental Science and Management,2013(2):120-123,127.
Authors:Li Zhongyu
Institution:Li Zhongyu(Putuo Environmental Monitoring Station,Shanghai 200062,China)
Abstract:This study optimized the preservation methods for 11 organophophorus pesticide samples in water. Water samples were stored at 4℃, and the spiked recoveries were determined by liquid - liquid extraction and GC/MS analysis. Water samples can be preserved for no more than 16 h without stabilizing agent. Solvents and pH regulating agents were added into water samples as stabilizing agents in a bid to extend the preservation time. The results showed that when 10 ml n - hexane and 10 ml acetic acid - sodium acetate buffer solution were added into 1 000 ml water sample as stabilizing agent, the preservation time can be extend- ed to 48 h. The effectiveness of this method was validated by surface water samples that were spiked at 0. 2μg/L and 0. 04μg/L, and the average spiked recoveries after 48 h were between 76. 2% and 95.0% with RSDs between 2. 4% and 7.2%.
Keywords:organophosphorus pesticides  water sample preservation  GC/MS
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