超声辅助提取高效液相色谱法检测小麦籽粒中杀雄嗪酸的残留  

Determination of Clofencet in Wheat Using Ultrasound-Assisted Extraction by High Performance Liquid Chromatography

作　　者：朱启迪[1] 张改生[1] 赵新亮[1,2] 张新钵[1] 杨书玲[1] 

机构地区：[1]西北农林科技大学,小麦育种教育部工程研究中心/陕西省作物杂种优势研究与利用重点实验室,杨凌712100 [2]河南科技学院生命科技学院,新乡453003

出　　处：《分析化学》2012年第3期462-465,共4页Chinese Journal of Analytical Chemistry

基　　金：国家“863”计划重大专项(Nos.2009AA101102,2011AA10A106);国家自然科学基金项目(Nos.31071477,31171611);高等学校博士学科点专项科研基金(No.20090204110024);陕西省“13115”科技创新工程重大科技专项(No.2014ZDKG-08)资助

摘　　要：建立了高效液相色谱法(HPLC)检测小麦籽粒中化学杂交剂SQ-1主成分杀雄嗪酸残留的方法。以75%乙醇为提取剂,正反萃取净化;采用Diamonsil C18不锈钢柱,以甲醇-0.5%(NH4)2HPO4溶液(60∶40,V/V,pH 2.5)为流动相,检测波长283 nm,流速1.0 mL/min。结果表明:化学杂交剂SQ-1主成分杀雄嗪酸在0.75～25.0 mg/L范围内线性关系良好,相关系数r=0.9999,在3个添加水平(1.0,5.0和10.0 mg/kg)范围内,平均加标回收率在84.2%～95.0%之间,相对标准偏差为1.0%～3.3%,检出限为0.075 mg/L。A method for the determination of the clofencet of chemical hybridizing agent SQ-1 in wheat has been established by high performance liquid chromatography.SQ-1 was extracted with 75% of ethanol and cleaned up by extraction and stripping technique.Diamonsil C18 column with the mobile phase consisted of methanol-water（60 ∶ 40,V/V,including 0.5% ammonium hydrogen phosphate,pH 2.5） at a flow rate of 1.0 mL/min was used for the detection at wavelength of 283 nm.A good linear relationship was obtained in the range of 0.75-25.0 mg/L with the correlation coefficient 0.9999.The average recoveries of SQ-1 were 84.2%-95.0%,the RSD were 1.0%-3.3%,and the detection limit was 0.075 mg/L.

关 键 词：小麦 高效液相色谱 正反萃取 化学杂交剂SQ-1 杀雄嗪酸 

分 类 号：S481.8[农业科学—农药学]