CAJ | 학술논문

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。
건립료일충이SAX고상소주췌취화고효액상색보（ HPLC）법동시검측토양중미서연산、갑기미초연、미초산갑지화미서을연산4충미서람동류제초제잔류적방법。고찰료불동제취제、pH、고상췌취（ SPE）소주화림세액체적등인소대회수솔적영향。결과표명：채용SAX 고상췌취소주，이V（을정）∶V（수）＝5∶3혼합용액위제취제，6 mL갑순위림세액시，재pH＝3조건하，양품적제취급정화효과교호。림출액농축후용갑순정용，과려막후경HPLC검측。첨가회수시험결과표명：재0?02～0．5 mg/kg첨가수평하，4충제초제적평균회수솔재86％～109％지간，상대표준편차（RSD）≤3．3％（n ＝5）。미서연산、갑기미초연화미서을연산재토양중적정량한（LOQ）균위0．01 mg/kg，미초산갑지적LOQ위0．02 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 ) .