摘要
目的建立超高效液相色谱-四极杆-飞行时间质谱法同时快速筛查与确证水果中11种常见农药残留的方法。方法建立11种农药的一级精确质量数据库和不同碰撞电压(10、20、40 V)条件下的二级谱库,采用QuEChERS方法对多种水果样品进行前处理,经优化的质谱和色谱条件上机,通过对比样品和数据库中一级精确质量、同位素分布与丰度以及保留时间进行初筛,再通过Target MS/MS数据与二级谱库进行比对确证,根据软件得分定性,外标法定量。结果11种农药在0.2~200.0μg/L范围内线性关系良好(r≥0.999),方法检出限在0.2~5.0μg/kg,低中高三个加标水平(5.0、10.0、50.0μg/kg)下的平均回收率(n=6)在91.2%~115.2%之间,精密度均小于15.0%。对60份水果样品进行筛查与确证,并依据《食品安全国家标准食品中农药最大残留限量》(GB 2763—2021)进行判定,均未超标。结论该方法具有高效率、高通量、高灵敏度等优点,且定量结果准确可靠,可以实现在较短时间及没有标准品的情况下对水果中常见11种农药的快速筛查。
Objective To establish a method for rapid screening and confirming 11 kinds of pesticide residues in fruit by ultra high performance liquid chromatography coupled with quadrupole time of flight mass spectrometry.Methods An accurate mass database at the first level and a fragment ion spectrum at the second level with 10,20,40 V were established.The various fruit samples were pretreated with QuEChERS method,and the optimized mass spectrometry and chromatography conditions were employed.The results were screened by comparing the accurate mass,isotope distribution and abundance,confirmed by comparing the Target MS/MS result in the database.The qualitative analysis was based on software scores,and the quantitative analysis used external standard method.Results There was good linear relationship for the 11 pesticides within the range of0.2-200.0μg/L(r≥0.999).The detection limit was between 0.2-5.0μg/kg.Adding low-level,medium-level and high-level standard(5.0,10.0,50.0μg/kg,respectively),the average recoveries(n=6)were between 91.2%-115.2%,and the relative standard deviations were less than or equal 15.0%.The method was applied to 60 samples of fruits for the screening and confirmation.None of pesticides exceeded the limit according to National Food Safety Standard-Maximum Residue Limits for Pesticides in Food(GB 2763-2021).Conclusions This method has the advantages of high efficiency,high throughput,and high sensitivity;the quantitative results are accurate and reliable;the 11 pesticides can be screened and confirmed in a short time and in the absence of standards.
作者
胡潇潇
杨妍
洪月玲
HU Xiaoxiao;YANG Yan;HONG Yueling(Zhengzhou City Center for Disease Control and Prevention,Zhengzhou,Henan 450000,China)
出处
《现代疾病预防控制》
2024年第4期275-279,共5页
MODERN DISEASE CONTROL AND PREVENTION
关键词
超高效液相色谱-四级杆-飞行时间质谱
水果
农药残留
Ultra high performance liquid chromatography coupled with quadrupole time of flight mass spectrometry
Fruit
Pesticide residues
