超高效液相色谱-串联质谱法快速测定果蔬中农药残留量的研究  

Rapid determination of pesticide residues in fruits and vegetables by UPLC-MS/MS method

作　　者：林守二 郑仁锦[1] 邱文倩[1] 诸寅 蔡佳玲 黄宏南[1] LIN Shou-er;ZHENG Ren-jin;QIU Wen-qian;ZHU Yin;CAI Jia-ling;HUANG Hong-nan(Fujian Center for Disease Control and Prevention,Fujian Provincial Key Laboratory of Zoonosis,Fuzhou,Fujian 350001,China;不详)

机构地区：[1]福建省疾病预防控制中心,福建省人兽共患病研究重点实验室,福建福州350001 [2]浙江清华长三角研究院

出　　处：《中国预防医学杂志》2020年第2期132-135,共4页Chinese Preventive Medicine

基　　金：福建省卫生计生科研人才培养项目(2017-1-26);浙江省科技计划项目(2018C37025)。

摘　　要：目的建立果蔬中15种农药残留的基质分散固相萃取-超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)快速分析方法。方法采集2018年市售果蔬样本,经1%乙酸-乙腈(V/V)提取,以MgSO4+PSA+C18为吸附剂的基质分散固相萃取净化,最后用C18柱分离,以乙腈和0.10%甲酸-5 mmol/L甲酸铵缓冲液作为流动相梯度洗脱分离,经串联质谱(MS/MS)电喷雾离子源(ESI)电离,多反应监测模式检测,基质匹配标准溶液外标法定量。结果15种农药组分的检测线性范围为0.5~200μg/L,检出限在0.114~0.391μg/kg,平均加标回收率在69.69%~106.41%,相对标准偏差在1.01%~8.15%。所采105份果蔬样本15种农药(多菌灵、嘧霉胺、啶虫脒、吡虫啉、甲霜灵、腐霉利、三唑酮、戊唑醇、丙环唑、甲基硫菌灵、咪鲜胺、烯酰吗啉、苯醚甲环唑、氯虫苯甲酰胺、茚虫威)检出率在0.95%~27.62%,但均未超过我国规定的农药最大残留限量值(GB 2763-2016)。结论UPLC-MS/MS简单、快速、有效,适合于果蔬中15种农药残留的快速检测。Objective To develop a rapid method for the determination of 15 pesticide residues in fruits and vegetables by matrix dispersive solid phase extraction and UPLC-MS/MS.Methods The samples collected in the market in 2018 were extracted by 1%acetic acid-acetonitrile(V/V),purified by matrix dispersive solid phase extraction with MgSO4+PSA+C18 as adsorbents and separated on C18 column with gradient elution using acetronitrile and 0.10%formic acid-5 mmol/L ammonium formate as mobile phase and detected by MS/MS using electrospray ionization(ESI)under the multiple reaction monitoring(MRM)mode,and quantified using external standard method with matrix matching standard solution.Results The linear range of 15 pesticide residues was between 0.5-200μg/L with the limit of detection(LOD)of 0.114-0.391μg/kg.The average recovery rates were in the range of 69.69%-106.41%with relative standard deviations(RSD)of 1.01%-8.15%.The detection rate of 15 pesticides(Carbendazim,Pyrimethanil,Acetamiprid,Imidacloprid,Metalaxyl,Procymidone,Triadimefon,Tebuconazole,Propiconazole,Thiophanate-methyl,Prochloraz,Dimethomorph,Difenoconazole,Chlorantraniliprole,Indoxacarb)in 105 samples ranged from 0.95%to 27.62%with none exceeding the maximum residue limit value(MRLs)specified in GB 2763-2016.Conclusions The method is simple,rapid and effective and it is suitable for the detection of 15 pesticide residues in fruits and vegetables.

关 键 词：超高效液相色谱-串联质谱 基质分散固相萃取 基质匹配 农药残留 

分 类 号：R155[医药卫生—营养与食品卫生学]