纤维微萃取联合气相色谱质谱法检测家禽饲料中有机磷农药残留  

Using fiber microextraction coupled with gas chromatography-mass spectrometry to detect residues of organophosphate pesticide in poultry feed

作　　者：马俊杰 宝泉 包沙日勒敖都 娜布其 赵璇 MA Junjie;BAO Quan;BAOSHA RileAodu;NA Buqi;ZHAO Xuan(Market Inspection and Testing Center in Tongliao City,Inner Mongolia,Tongliao 028000,China)

机构地区：[1]通辽市市场检验检测中心,内蒙古通辽028000

出　　处：《养殖与饲料》2024年第12期18-22,共5页Animals Breeding and Feed

摘　　要：[目的]为了更好地检测家禽饲料中常见的有机磷农药残留,优化并提高对家禽饲料样品中有机磷农药萃取后的回收率。[方法]采用固相纤维微萃取技术搭配气相色谱-质谱联用分析,通过改变搅拌速度、提取时间、pH值、无机盐的添加、解析溶剂与解析溶剂体积等各萃取试验参数,对家禽饲料中氯吡硫磷、马拉硫磷、特丁磷和三唑磷四类有机磷农药的萃取效率进行了优化试验。[结果]采用优化后的萃取方法,家禽饲料中有机磷农药的回收率为91.8%~98.3%。在试验条件为搅拌速度1200 r/min、提取时间25 min、pH值为6、乙酸乙酯重复2次解吸且未添加其他盐类的情况下,有机磷农药的提取效率较高,达98.3%。[结论]优化后的固相纤维萃取方法具有高灵敏度和良好的重复性,绿色、快速、经济可行性等特点,大大提升了家禽饲料样品中有机磷农药的检测分析萃取效率。[Objectives]The recovery rate of organophosphate pesticides extracted from samples of poultry feed was optimized and improved to better detect residues of common organophosphate pesticide in poultry feed.[Methods]Solid phase fiber microextraction coupled with gas chromatography-mass spectrometry was used to optimize the extraction efficiency of four types of organophosphate pesticides including clopyralid,malathion,terbufos and triazophos in poultry feed by changing parameters of extraction including stirring speed,extraction time,pH,addition of inorganic salts,and resolving solvents and volume of resolving solvents.[Results]The recovery rate of organophosphate pesticides in poultry feed with the extraction method optimized was in the range of 91.8%to 98.3%.The extraction efficiency of organophosphate pesticides was the highest,reaching 98.3%under the experimental conditions of stirring speed of 1200 r/min,extraction time of 25 min,pH6,repeated desorption of ethyl acetate twice without adding other salts.[Conclusions]The optimized solid phase fiber extraction method has the characteristics of high sensitivity,good repeatability,green,rapid,and economical feasibility,greatly improving the efficiency of detecting,analyzing,and extracting organophosphate pesticides in samples of poultry feed.

关 键 词：饲料安全 饲料检测 有机磷农药 农药残留 固相纤维微萃取技术 气相色谱-质谱 

分 类 号：S816.17[农业科学—饲料科学]