摘要
为解决有机磷农药残留量检测分析过程中基质效应影响检测结果的问题,本研究以电喷雾(ESI)为离子源,正离子模式多级反应离子检测(MRM)方式,建立了一种灵敏度高、选择性强的基质校正液相色谱-串联质谱法(LC-MS/MS),以同时测定洋葱、葱、姜、蒜及韭菜中28种有机磷农药残留量。以洋葱为试材,优化选择了乙酸/乙腈(1:100Vol)+6 g氯化钠为最佳提取体系,并确定超声提取30 min、快速混匀器振荡1.5 min为最佳提取条件。利用该方法检测洋葱28种有机磷农药含量,在0.200~100μg·L^(-1)质量浓度范围内其与峰面积之间呈线性关系,相关系数为0.99827~0.99990;方法检出限0.06~0.89μg·kg^(-1),定量限0.24~3.6μg·kg^(-1);28种有机磷农药残留量在10.0,50.0,200μg·kg^(-1)3个浓度水平的平均回收率为76.4%~102.6%,相对标准偏差为1.1%~9.0%。利用该方法检测葱、姜、蒜及韭菜中28种有机磷农药残留量在10μg·kg^(-1)浓度水平的平均回收率为74.7%~109.9%,相对标准偏差为0.61%~6.2%。综合而言,所建立的新方法能满足实际样品分析检测的要求。
In order to solve the matrix effect in the detection process,the experiment developed a highly sensitive,selective,and matrix corrected LC-MS/MS method by electrospray ionization(ESI)as ion source and MRM in positive ion mode,which could simultaneously determine 28 organophosphorus pesticide residues of onion,scallion,ginger,garlic and leek.Using onion as material,the conditions of HPLC and MS for determination of 28 organophosphorus pesticides were optimized,the optimal extraction system were acetic acid/acetonitrile(1:100Vol)+6 g NaCl,and the optimal extraction process were 30 min of ultrasonic extraction and 1.5 min rapid mixer oscillation.The above method were used to detect the 28 organophosphorus pesticides in onion,there was a good linear relationship between the organophosphorus pesticides content and peak area in the range of 0.200^(-1)00μg·L^(-1),and the correlation coefficients were 0.99827-0.99990;the detection and quantitation limit were in the range of 0.06-0.89μg·kg^(-1) and 0.24-3.6 g·kg^(-1),respectively;the recovery rate of 28 organophosphorus pesticides residues for 10,50,200μg·kg^(-1) levels ranged from 76.4%to 102.6%,which the relative standard deviation were ranged from1.1%to 9.0%.The above method were used to detect the 28 organophosphorus pesticides residues in scallion,ginger,garlic,and leek,the recovery rate for 10μg·kg^(-1) level were ranged from 74.7%to 109.9%,which the relative standard deviation were ranged from 0.61%to 6.2%.Comprehensively,the new method could meet the requirements of actual sample analysis.
作者
王孝钢
范津珲
江志训
刘彩飞
WANG Xiaogang;FAN Jinhui;Jiang Zhixun;LIU Caifei(Qingdao Academy of Agricultural Sciences,Qingdao,Shandong 266109,China;Agricultural and Rural Bureau of Jimo District,Qingdao,Shandong 266200,China)
出处
《天津农业科学》
CAS
2021年第12期63-73,共11页
Tianjin Agricultural Sciences
关键词
液相色谱-串联质谱法
有机磷农药
洋葱
葱
姜
蒜
韭菜
LC-MS/MS
organophosphorus pesticide residues
onion
scallion
ginger
garlic
leek
