北京市疾病预防控制中心 食物中毒诊断溯源技术北京市重点实验室,北京 100013
张 晶,研究员,研究方向:食品中危害因子的非定向筛查、精准检测及评估,E-mail:brightjing@163.com
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郭巧珍,杨奕,刘丽萍等.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[J].分析测试学报,2023,42(10):1242-1250.
GUO Qiao-zhen,YANG Yi,LIU Li-ping,et al.Screening of Pesticides in Fresh Peach by QuEChERS Combined with Ultra-high Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(10):1242-1250.
郭巧珍,杨奕,刘丽萍等.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[J].分析测试学报,2023,42(10):1242-1250. DOI: 10.19969/j.fxcsxb.23070601.
GUO Qiao-zhen,YANG Yi,LIU Li-ping,et al.Screening of Pesticides in Fresh Peach by QuEChERS Combined with Ultra-high Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(10):1242-1250. DOI: 10.19969/j.fxcsxb.23070601.
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-QTOF MS)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-QTOF MS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-QTOF MS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 pesticides 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 others were herbicides and plant growth regulators. All samples were detected with one or more pesticides,of which 18 pesticides had national limit standards. The antibacterial carbendazim and flusilazole 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. Multiresidues of pesticides in peach samples were ubiquitous,thus,more relevant residues monitor and health risk assessment should be conducted in the future.
鲜桃农药残留超高效液相色谱-四极杆-飞行时间质谱
fresh peachpesticidesultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry
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