液相色谱-高分辨飞行时间质谱法快速筛查食品中香港规例农药残留  

Rapid Screening and Confirmation of Residue Compounds in Foods from Regulation of Pesticides in Hong Kong by Liquid Chromatography Coupled with High Resolution Quadrupole Time-of-Flight Mass Spectrometry

作　　者：潘孝博 伊雄海[2] 时逸吟 赵善贞[2] 盛永刚[2] 邓晓军[2] 朱坚[2] 丁卓平[2] 

机构地区：[1]上海海洋大学食品学院,上海201306 [2]上海出入境检验检疫局,上海200135

出　　处：《分析化学》2016年第7期1125-1132,共8页Chinese Journal of Analytical Chemistry

基　　金：上海出入境检验检疫课题(Nos.HK008-2015;HK005-2015);上海市技术性贸易措施应对专项(Nos.14TBT006;15TBT004;15TBT005);上海市技术标准专项(No.15DZ0503201)资助

摘　　要：建立了液相色谱-四级杆串联飞行时间质谱法测定食品中249种香港《食物内残余除害剂规例》农药残留的筛查方法。样品经1%甲酸-乙腈提取,改进的Qu ECh ERS方法提取净化,Agilent Poroshell 120 EC-C18色谱柱（150 mm×3 mm i.d.,2.7μm）分离,流动相为0.1%甲酸水和甲醇溶液,梯度洗脱,电喷雾离子源,正模式下侦测,建立了一级精确质量和二级碎片离子质谱数据库,并且对11种典型食品的基质效应进行考察,基质匹配外标法定量。结果表明,在10-500μg/kg浓度范围内,249种目标化合物线性关系良好（r〉0.99）,方法定量限为10-100μg/kg（S/N≥10）,在大米、香菇、黄豆、菠菜、西红柿、西兰花、柚子、韭菜、胡萝卜、生菜、黄瓜中3个添加水平的平均回收率范围分别为23.2%-133.2%,35.6%-137.6%和38.7%-140.2%,相对标准偏差（RSD）在1.3%-19.2%之间（n=6）。方法操作简便,耗时短,灵敏度高,稳定性好,用于日常筛查检测可显著降低检测成本,具有实际应用价值。A method for screening of 249 residue compounds of pesticide in foods from the Hongkong＇s regulation was developed by liquid chromatography coupled with quadrupole time-of-flight mass spectrometry （LC-Q-TOF/MS）. The target analytes were dissolved in acetonitrile with 1% formic acid, then extracted and purified by using a modified QuEChERS method. The chromatographic separation was performed on an Agilent Poroshell 120 EC-C18 column （ 150 mm×3 mm i. d., 2.7 μm） with gradient elution using 0. 1% （V/V） formic acid and methanol as mobile phase. The target compounds were monitored under positive ionization mode with ESI source. The matrix effects in 11 kinds of typical foods were considered and the quantification was carried out by matrix-matched with external standard method. Two databases of accurate mass and fragment ions were created. The results demonstrated that the linear range was from 10 μg/kg to 500 μg/kg with good correlation coefficients （ r 〉 0. 90 ）. The method quantitation limits were in the range of 10 - 100 μg,/kg （S/N≥10）. For rices, mushrooms, soybeans, spinaches, tomatoes, broccolies, grapefruits, chives, carrots, lettuces and cucumbers, the average recoveries at three spiked levels were in the range of 23.2% -133.2%, 35.6% -137.6%, and 38.7% -140.2%, and the relative standard deviations （RSDs） were 1.3%-19.2% （n = 6）. The method is simple, time-saving with high sensitivity and good reproducibility, as well as having practical application for its low test cost.

关 键 词：液相色谱-四级杆串联飞行时间质谱法 筛查 农药残留 

分 类 号：O657.63[理学—分析化学] TS207.53[理学—化学]