摘要
提出了气相色谱法测定水中10种不同极性有机磷农药含量的方法。取水样50 mL,用盐酸(1+1)溶液调节其酸度至pH 3~5,过LiChrolut EN Merck固相萃取小柱,先后用丙酮2 mL、乙腈2 mL、二氯甲烷2 mL作为洗脱剂进行洗脱,再经石墨化炭黑柱净化。用乙腈及丙酮各3 mL淋洗炭黑柱,洗脱液供GC分析。采用DB 17毛细管色谱柱分离,火焰热离子检测器测定。10种有机磷农药的线性范围均在0.1~4.0μg·L^(-1)之间,方法的检出限(3s)在0.10~0.30μg·L^(-1)之间。方法用于测定水样中有机磷农药的含量,并进行加标回收试验,回收率在78.8%~102%之间,测定值的相对标准偏差(n=7)在1.7%~7.4%之间。
A method of GC for the determination of 10 organophosphorus pesticides with different polarity in water was proposed. Acidity of water sample （50 mL） was adjusted to pH 3--5 with HCI （1＋1 ） solution, and the sample solution was extracted on I.iChrolut EN Merck solid phase extraction column （SPE）. Then organophosphorus pesticides on the SPE column were eluted in succession with acetone （2 mL）, acetonitrilc （2 mL） and CH2Cl3 （2 mL）; and the eluate obtained was purified on graphitized carbon black column. The carbon black column was eluted with 3 mL each of acetonitrile and acetone, and the eluate was used for GC analysis. I）}317 capillary column was used for separation, and FTD was used for determination. I.inearity ranges for the 10 organophosphorus pesticides were found to be same between of 0. 1 4.0 μg·L^-1 , with detection limit （3s） in the range of 0. 10 0. 30μg·L^-1.The proposed method was applied to the determination of organophosphorus pesticides in water sample, giving values of recovery by standard addition method in the range of 78. 8G 102% with RSDrs （n=7） in the range of 1.7%-7.4%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2013年第7期820-823,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
中国地质科学院水文地质环境地质研究所基本科研业务费(SK201204)
地质调查项目(G201120)资助
关键词
固相萃取
气相色谱法
有机磷农药
水
Solid phase extraction
GC
Organophosphorus pesticides
Water
