食品中27种农药残留量的高效液相色谱-串联质谱测定法  

Determination of 27 Kinds of Pesticide Residues in Food by LC/MS

作　　者：于红卫[1] 曲青[1] 郝文[1] 

机构地区：[1]山东省青岛市疾病预防控制中心理化科,266033

出　　处：《职业与健康》2011年第23期2704-2706,共3页Occupation and Health

摘　　要：目的建立以固相萃取/高效液相色谱-串联质谱(LC/MS)同时测定食品中27种农药残留量的方法。方法采用酸性乙腈匀浆提取。盐析离心后,过C18柱净化去脂,经LC/MS电喷雾电离(ESI)源,负离子多反应(MRM)模式检测,外标法定量。用乙腈-酸性水(pH=5)作为流动相,梯度洗脱,根据不同检测要求用液相色谱-串联质谱仪检测农药多残留组分。结果所有27种农药均在40 min内流出,农药标准的线性范围在0.05～10.0μg/ml,相关系数r均在0.99以上,低、高2种浓度加标回收率均在80.2%～96.2%之间,相对标准偏差均小于10%,方法最低检出限在0.001～0.040 mg/kg(S/N=3)。结论方法简单、快速、灵敏,适合于食品中有机磷、有机氯、拟除虫菊酯、氨基甲酸酯、除草剂等农药残留的测定,且准确度好,精密度高,适用于食品中27种农药同时分析。[Objective]To establish the method for simultaneous determination of 27 kinds of pesticide residues by solid-phase extraction-LC/MS.[Methods]This method adopted acidic acetonitrile homogenate extraction.After salting-out centrifugation,the sample was degreased and purified through C18 pillar,then detected through LC-ESI-MS/MS,MRM.Acidic acetonitrile（pH=5） was used as mobile phase and gradient elution,the multicomponent pesticide residues can be detected by LC/MS based on different detection request.[Results]The 27 kinds of pesticides all outflowed in 40 minutes.The linear rang of pesticide standard was 0.05~10.0 μg/ml and the correlation coefficient r was all above 0.99.The recoveries at high and low concentrations was between 80.2%~96.2%.The relative standard deviation was within 10% and the method of the lowest detection was 0.001~0.040 mg/kg（S/N=3）. [Conclusion]This method is simple,rapid,sensitive and suitable for pesticide residue detection for organophosphoms,organochlorine,pyrethroid,carbamate,herbicide in food.And the method has better accuracy,high precision,can be used for simultaneous determination of 27 pesticides in food.

关 键 词：食品 农药 液相-质谱 选择离子监测方式 

分 类 号：R115[医药卫生—公共卫生与预防医学]