QuEChERS/超高效液相色谱-四极杆-飞行时间质谱法筛查鲜桃中的农药残留

Screening of Pesticides in Fresh Peach by QuEChERS Combined with Ultra-high Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry

采用QuEChERS前处理技术结合超高效液相色谱-四极杆-飞行时间质谱(UPLC-QTOFMS)筛查了鲜桃中的农药残留。鲜桃均质后经1%乙酸乙腈提取,加入无水醋酸钠和无水硫酸镁,以PSA和石墨化炭黑(Carb)净化,利用UPLC-QTOFMS进行数据采集,经UNIFI软件进行峰谱识别后,利用自建农药谱库进行检索筛查。在23份鲜桃中检出33种农药,其中杀虫剂占49%,抗菌剂占33%,其余为除草剂和植物生长调节剂。所有样本中均筛查出一种或多种农药,其中18种农药有国家限量标准,2份鲜桃中的抗菌剂多菌灵和氟硅唑分别超过标准限量。研究表明UPLC-QTOFMS高分辨质谱技术是筛查水果中农药残留的有效手段,鲜桃中存在多种农药残留,需进一步对其残留水平和暴露风险进行研究。

QuEChERS combined with ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry(UPLC-QTOF MS)method was developed for the screening of pesti-cides in peach.Homogeneous fresh peach samples were extracted by acetonitrile containing 1%acetic acid,added with anhydrous sodium acetate and anhydrous magnesium sulfate,purified by PSA and Carb dispersion solid phase extraction powder,and then analyzed using UPLC-QTOF MS under data independent acquisition mode and screened by a self-built pesticides library.Peak identification and spectrum library retrieval were carried out by the UNIFI software.33 pesticides were detected in 23 fresh peach samples,of which 49%were insecticides,33%were antibacterial agents,and the oth-ers were herbicides and plant growth regulators.All samples were detected with one or more pesti-cides,of which 18 pesticides had national limit standards.The antibacterial carbendazim and flusi-lazole in 2 fresh peach samples were exceeded the maximum residue limit.This study indicated that UPLC-QTOF MS screening is an effective analytical method to detect pesticides in fruits.Multiresi-dues of pesticides in peach samples were ubiquitous,thus,more relevant residues monitor and health risk assessment should be conducted in the future.