摘要
建立了同时检测对土壤中磺胺脒、磺胺嘧啶、磺胺甲恶唑、烯啶虫胺、吡虫啉、噻虫啉、多菌灵7种农药残留的在线净化-双检测器-高效液相色谱新方法。实验对提取净化和分析条件进行了优化,得出最佳实验条件:土壤样品经提取液(甲醇:乙腈:二氯甲烷=5:4:1,V/V/V)提取,氮吹浓缩后直接进样,经在线固相萃取(SPE)柱在线净化,梯度洗脱经反相C18色谱柱分离,二极管阵列(DAD)检测器串联荧光(FLD)检测器检测,外标法定量,12 min内即可完成7种农兽药的检测。7种农药检出限为1.1~3.0×10^(-3)mg/kg(S/N=3),线性范围内线性相关系数均在0.9999以上。空白土壤样品在0.05,0.10,0.32 mg/kg添加水平的平均加标回收率为71.92%~103.88%,相对标准偏差为0.07%~4.1%。
In this research,seven pesticide residues in soil,including carbendazol,thiacloprid,imidacloprid,sulfamethoxaz,nitenpyram,sulfadiazine and sulphaguanidine,have been concentrated and detected with online solid phase extraction-high performance liquid chromatography（ SPE-HPLC） method. Both of online-SPE concentration and parameter determination of HPLC-DAD / FLD have been optimized to get the best experimental conditions： the target compounds in soil samples were extracted by the mixed solution of methyl alcohol,acetonitrile and dichloromethane（ 5： 4： 1,V / V / V） under ultrasonic operation,concentrated by nitrogen gas,purified with a PEP on-line SPE column（ Hyper Sep Retain PEP,5 μm,10 mm × 3 mm） and finally analyzed by column（ Diamonsil C185μm,250 mm × 4. 6 mm） at gradient elution mode with methanol as mobile phase. Analytes were determined using DAD and FLD detector and quantified by external standard method. The detection limits were 1. 1 - 3. 0 × 10^-3mg / kg（ S / N = 3）,and seven residues had good linear responses（ R〉0. 9999）. The recoveries at low,medium and high concentration levels were 71. 9% - 103. 9%,while RSDs were 0. 07% -4. 1%. The method is simple,rapid and highly efficient,which has been successfully utilized to detect seven residues in soil and would improve soil treatment techniques in the future.
出处
《分析试验室》
CAS
CSCD
北大核心
2016年第8期874-879,共6页
Chinese Journal of Analysis Laboratory
基金
国家自然科学基金项目(81573202
81402723)
河北省食品药品监督管理局科技项目(Pt 2014043)资助
关键词
在线净化-高效液相色谱
紫外和荧光检测器
多菌灵
磺胺类药物
新烟碱类农药
土壤
On-line solid phase extraction-high performance liquid chromatography
DAD and FLD detector
Sulphaguanidine
Sulfonamides
Neonicotinoid pesticide residues
