液相色谱-串联质谱检测土壤和大豆中咪唑乙烟酸的残留  

Determination of Imazethapyr Residues in Soil and Soybean by HPLC-MS/MS

作　　者：贾福艳[1] 王娇[1] 蒋培宇 刘永利[1] 黄成田[1] 赵凌菲[1] 黄鑫[1] 丁琦[1] 

机构地区：[1]沈阳化工研究院有限公司,辽宁沈阳110021

出　　处：《农药科学与管理》2017年第12期20-24,共5页Pesticide Science and Administration

摘　　要：建立液相色谱-串联质谱(HPLC-MS/MS)测定土壤、大豆植株、毛豆和黄豆中咪唑乙烟酸的残留分析方法。土壤中咪唑乙烟酸经pH=10的氯化铵-氨水缓冲溶液超声提取,调pH至酸性后再经二氯甲烷萃取,HPLC-MS/MS检测;大豆植株、毛豆及黄豆中咪唑乙烟酸经乙腈(含1%甲酸):水(含1%甲酸)=80:20(v/v)混合溶液超声提取,SPE-C_(18)固相萃取柱净化,HPLC-MS/MS检测。咪唑乙烟酸在所有样品中的平均添加回收率为81.0%～104.2%,相对标准偏差为1.4%～10.4%。方法的最小检出质量分数(LOQ)为0.01～0.02mg/kg。该方法选择性好、灵敏度高,适合于土壤、大豆植株、毛豆和黄豆中咪唑乙烟酸的残留检测。A HPLC - MS/MS method for determination of Imazethapyr residues in soil, plant, green soybean and soybean samples was developed. The soil samples were firstly extracted with Am- monia Chloride- Ammonium Hydroxied （pH = 10） buffer solution by uhrasonication. After adjus- ted to be acidic, the solution was re -extracted with dichloromethane. The plant, green soybean and soybean samples were extracted with acetonitrile （containing 1% formic acid） ： water （contai- ning 1% formic ac cleaned up by SPE id） -C = 80： 20 （v/v） solution by ultrasonication. The extracted solution was 18 and analyzed by HPLC - MS/MS. The average recoveries of imazethapyr in different type of samples were at the range of 81.0% to 104.2%, and the relative standard devia- tions （RSDs） were 1.4% to 10.4%. The limit of quantifications （LOQs） were 0.01 - 0. 02mg/ kg. The method is characterized by good sensitivity and accuracy, which is suitable for the determi- nation of imazethapyr residue in soil, plant, green soybean and soybean samples.

关 键 词：咪唑乙烟酸 液相色谱-串联质谱 残留分析 土壤 大豆 

分 类 号：S481.8[农业科学—农药学]