摘要
目的应用超高效液相色谱-四级杆飞行时间质谱技术建立一种对果蔬中40种农药残留进行快速筛查的方法。方法采用分散固相萃取方法对果蔬样品进行前处理,BEH C18色谱柱(2.1 mm×100 mm,1.7μm)分离,以乙腈/含5 mmol/L甲酸铵的0.1%甲酸水溶液为流动相进行梯度洗脱,在优化后的质谱参数下进行测定。同时建立40种农药在此条件下的一级精确质量数据库和不同碰撞电压(5/10/20/30/40 V)条件下的二级谱库,通过自建谱库对样品中农药进行快速筛查,基质匹配外标法定量。结果该方法可以对果蔬中40种农药进行准确定性和定量,各种类农药的线性相关系数均大于0.9950,方法检出限在0.05~7μg/kg,3个加标水平下的平均回收率(n=6)在79.3%~120.0%之间,精密度均小于10%。采用此方法对24份样品进行筛查与确证,其中22份样品中检出噻虫嗪、吡唑醚菌酯、噻虫胺、烯酰吗啉等多种农药残留。结论该方法简单快速,其建立的谱库可以实现没有标准品的情况下对果蔬中40种农药进行快速筛查。
Objective To develop a method for the rapid screening 40 types of pesticide residues in fruits and vegetables using ultra high performance liquid chromatography(UHPLC)coupled with quadrupole time of flight mass spectrometry(QTOF-MS).Methods Fruit and vegetable samples were pretreated using QuEChERs method and separated on a BEH C18 column(100 mm×2.1 mm,1.7μm)with acetonitrile as the organic phase and 0.1%formic acid/5 mmol/L ammonium formatted as the aqueous phase.Detection was performed under the optimized MS conditions.An accurate mass database and a fragment ion spectra were established with voltages of 5,10,20,30,and 40 V.Results were screened by comparing against a self-built pesticides database and quantified using the matrix matching method.Results The method established can accurately identify and quantify 40 types of pesticides in fruits and vegetables.The correlating coefficient of the calibration curves for pesticides exceeded 0.9950,and the detection limits ranged from 0.05 to 7μg/kg.The average recoveries were in the range of 79.3%to 120.0%at three spiking levels,with relative standard deviations less than 10%.The method was applied to analyze 24 samples of fruits,in which 22samples were found to contain multiple pesticide residues such as thiacloprid,pyraclostrobenz,imidacloprid,and propiconazole.Conclusion This method is simple and rapid,and the established spectral library enables rapid screening of 40 types of pesticides in fruits and vegetables without the need of standard products.
作者
胡潇潇
杨妍
程名玉
杜利敏
李志岭
HU Xiaoxiao;YANG Yan;CHENG Mingyu;DU Limin;LI Zhiling(Zhengzhou City Center for Disease Control and Prevention,Zhengzhou 450000,China)
出处
《现代疾病预防控制》
2025年第1期62-68,共7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
快速筛查
果蔬
农药残留
Ultra high-performance liquid chromatography
Quadrupole time-of-flight mass spectrometry
Rapid screening
Fruits and vegetables
Pesticide residues
作者简介
通信作者:胡潇潇,主管技师,硕士,研究方向:卫生理化检验,E-mail:1009808770@qq.com。
