反相高效液相色谱法测定生活饮用水中氨基甲酸酯农药残留  

Determination of carbamate pesticide residues in drinking water by reversed phase high performance liquid chromatography

作　　者：卢忠魁[1] 常海华[1] 尚轶[1] 邱宇鹤 张特[1] 

机构地区：[1]吉林市疾病预防控制中心,吉林吉林132001

出　　处：《中国卫生检验杂志》2015年第21期3617-3619,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的研究应用反相高效液相色谱荧光检测器直接测定生活饮用水中氨基甲酸酯农药残留量的方法。方法采用Oasis HLB固相萃取柱富集浓缩生活饮用水中的氨基甲酸酯农药,柱温为40℃,以甲醇-水(55∶45,V/V)为流动相进行等度洗脱,流速为1.00 ml/min,以Symmetry C18柱(4.6 mm×250 mm,5μm)为分析柱,采用荧光检测器直接测定生活饮用水中氨基甲酸酯农药的含量,无需柱后衍生设备进行化学衍生化反应。结果当呋喃丹、甲萘威的浓度为0.050μg/ml^10.00μg/ml时,线性关系良好,相关系数(r)>0.999。检出限分别为0.16μg/L、0.07μg/L。在高、中、低3种浓度水平下,呋喃丹、甲萘威的平均加标回收率分别为89.4%~90.9%、90.5%~93.6%,相对标准偏差(RSD)分别为3.72%~8.50%、4.35%~7.14%。结论应用研究的新方法能够满足生活饮用水中氨基甲酸酯农药残留量的测定要求,方法简便、准确、快速、高效,易于在基层实验室实施。Objective To develop a reversed phase high performance liquid chromatography（ HPLC） method for the detection of carbamate pesticides in drinking water. Methods The drinking water were extracted by Oasis HLB solid phase extract cartridge and tested under the following conditions,column temperature was 40 ℃; mobile phase was methanol- water（ 55∶45,V / V）,elution flow equal degree at 1. 00 ml / min for isocratic elution; Symmetry C18column（ 4. 6 mm × 250 mm,5 μm） as the analysis column; direct determination of the content of urethane pesticides in drinking water was conducted by fluorescence detector without deriving equipment for chemical derivatization reaction after column elution. Results The linear range was among 0. 050 μg / mg-10. 00 μg / mg for carbofuran and carbaryl,there was good linearity with the correlation coefficient（ r） 0. 999. The detection limit was respectively 0. 16 μg / L and 0. 07 μg / L. Average recoveries of spiked standard materials at three quantity levels of carbofuran and carbaryl were 89. 4%- 90. 9% and 90. 5%- 93. 6%. The relative standard deviation was among 3. 72%- 8. 50% and4. 35%- 7. 14%. Conclusion The method can meet the detection need of the amount of carbamate pesticide residues in drinking water,and is simple,accurate,fast and efficient,and easy to be applied in primary laboratories.

关 键 词：液相色谱 生活饮用水 农药 固相萃取 

分 类 号：O657.72[理学—分析化学]