建立了一种以SAX固相小柱萃取和高效液相色谱( HPLC)法同时检测土壤中咪唑烟酸、甲基咪草烟、咪草酸甲酯和咪唑乙烟酸4种咪唑啉酮类除草剂残留的方法。考察了不同提取剂、pH、固相萃取( SPE)小柱和淋洗液体积等因素对回收率的影响。结果表明:采用SAX 固相萃取小柱,以V(乙腈)∶V(水)=5∶3混合溶液为提取剂,6 mL甲醇为淋洗液时,在pH=3条件下,样品的提取及净化效果较好。淋出液浓缩后用甲醇定容,过滤膜后经HPLC检测。添加回收试验结果表明:在0?02~0.5 mg/kg添加水平下,4种除草剂的平均回收率在86%~109%之间,相对标准偏差(RSD)≤3.3%(n =5)。咪唑烟酸、甲基咪草烟和咪唑乙烟酸在土壤中的定量限(LOQ)均为0.01 mg/kg,咪草酸甲酯的LOQ为0.02 mg/kg。
A new method for determining residues of imazapyr, imazapic, imazamethabenz-methyl and imazethapyr in soil was developed by solid-phase extraction ( SPE ) cleanup and high performance liquid chromatography( HPLC) detection. Various extraction reagents, solvents at different pH values, various type of SPE and the elution volumes were compared. Extraction with V ( acetonitrile )∶V(water) =5∶3 at pH 3, with SAX cartridge SPE purification of the extracts were found to be the most suitable conditions. Determination was done with HPLC coupled with diode array detector ( DAD ) . Mean recoveries of four imidazolinone herbicides at fortification levels of 0 . 02-0 . 5 mg/kg were between 86% -109% (RSD≤3. 3%, n=5). Under the optimal conditions, limits of quantification in soil were 0?01 mg/kg for imazapyr, imazapic and imazethapyr, and 0. 02 mg/kg for imazamethabenz-methyl ( S/N=3 ) .