节点文献
气相色谱法测定复杂基质蔬菜中11种农药的残留量
GC Determination of Residual Amounts of 11 Pesticides in Vegetables of Complex Matrixes
【摘要】 葱、姜、蒜、洋葱、韭菜、蒜苔等复杂基质蔬菜样品中六六六、滴滴涕、四氯硝基苯、五氯硝基苯、艾氏剂等11种农药残留用丙酮-正己烷(1+1)混合溶剂均质提取,加入20 g.L-1硫酸钠溶液用正己烷进行液-液分配,提取液用浓硫酸净化后所得有机相在13 kPa压力条件下进行旋转蒸发至近干,用正己烷使残渣溶解并定容为1.0 mL,用于气相色谱法测定。采用DB-1701毛细管柱分离,用气相色谱-微池电子捕获检测器检测,在2个不同浓度水平上加入11种农药混合标准溶液进行回收试验,测得其回收率在81.6%~97.1%之间,测定值的相对标准偏差(n=6)均小于7.5%。该方法的检出限(3S/N)为0.5μg.kg-1。
【Abstract】 Eleven pesticides of residual amounts(including BHC,DDT,tecnazene,quirtozene,aldrin and etc.) were extracted from samples of vagetables of complex matrixes with mixed solvent of acetone and n-hexane(mixed in the ratio of 1 to 1 by volume),and partitioned with 20 g·L-1 Na2SO4 solution.The n-hexane extract was purified by shaking with conc.H2SO4.After removing the H2SO4 phase,the hexane phase was washed with 20 g·L-1 Na2SO4 solution,and dehydrated with anhydrous Na2SO4.Then the solution in n-hexane was evaporated to near dryness by rotary evaporation under 13 kPa.The residue was taken and made up to 1.0 mL with n-hexane and used for GC determination.After separation on the DB 1701 capillary column,GC determination was carried out with μ-ECD.Recovery tests were made at 2 concentration levels by addition of mixed standard solution of the 11 pesticides to 4 kinds of vegetables as the matrixes,results of recovery found were in the range from 81.6% to 97.1%,with RSD′s(n=6) less than 7.5%.Detection limit(3S/N) of the method found was 0.5 μg·kg-1.
【Key words】 GC; Complex matrix vegetables; Organochlorines pestcides; Residue analysis;
- 【文献出处】 理化检验(化学分册) ,Physical Testing and Chemical Analysis(Part B:Chemical Analysis) , 编辑部邮箱 ,2009年07期
- 【分类号】TS255.7
- 【被引频次】13
- 【下载频次】198