阵列式薄膜固相微萃取结合高效液相色谱-串联质谱法测定农产品中13种农药残留

Determination of 13 kinds of pesticide residues in agricultural products by array-thin film micro-extraction coupled with high performance liquid chromatography-tandem mass spectrometry

中文关键词:  阵列式薄膜固相微萃取  样品前处理  高效液相色谱-串联质谱法  农药残留

英文关键词:array-thin film micro-extraction  sample pretreatment  high performance liquid chromatography- tandem mass spectrometry  pesticide residues

中文摘要:

      目的 建立阵列式薄膜固相微萃取(array-thin film micro-extraction, aTFME)结合高效液相色谱-串联三重四极杆质谱法检测农产品中13种农药残留的分析方法。方法 将样品粉碎匀浆, 以聚丙烯腈-亲疏水平衡材料(polyacrylonitrile-hydrophile lipophile balance, PAN-HLB)作为aTFME薄膜材料振荡吸附30 min后, 加入洗脱液(乙腈:甲醇:水=17:2:1, V:V:V)振荡洗脱30 min, 采用Agilent Poroshell 120 EC-C18色谱柱(150 mm× 3.0 mm, 2.7 μm)分离, 以甲醇和0.1%甲酸溶液体系为流动相进行梯度洗脱, 电喷雾离子源正离子扫描, 多反应监测模式检测, 基质匹配标准曲线法定量。结果 13种农药化合物在一定浓度范围内线性关系良好(r2>0.99); 在梨、大白菜、茶样品中检出限和定量限范围分别为0.08~1.20 μg/kg和0.20~4.00 μg/kg; 选择空白样品在低、中、高3个水平进行添加回收实验, 3种样品回收率分别为70%~114%、72%~121%、70%~121%。结论 本研究应用的aTFME前处理技术具有操作简便、效率高、有机试剂消耗低、可重复利用、灵敏度高的优势, 可为农产品中农药的检测提供技术支持。

英文摘要:

      Objective To establish a method for the determination of 13 kinds of pesticide residues in agricultural products by array-thin film micro-extraction (aTFME) combined with high performance liquid chromatography-tandem triple quadrupole mass spectrometry. Methods The samples were crushed and homogenized, and the polyacrylonitrile-hydrophile lipophile balance (PAN-HLB) was prepared as aTFME film material for oscillating adsorption for 30 min, the eluent (acetonitrile:methanol:water=17:2:1, V:V:V) was added to shake and elute for 30 min. Utilizing Agilent Poroshell 120 EC-C18 chromatographic column (150 mm×3.0 mm, 2.7 μm) to separate, using methanol and 0.1% formic acid solution system as mobile phase for gradient elution, electrospray ion source positive ion scanning, multiple reaction monitoring mode detection, matrix-matched standard curve method for quantification. Results The 13 kinds of pesticide compounds had a good linear relationship in a certain concentration range (r2>0.99); the limits of detection and quantification in pear, Chinese cabbage and tea samples range from 0.08 to 1.2 μg/kg and 0.20 to 4.00 μg/kg; the recovery experiments were performed at low, medium and high levels utilizing standard sample spiked into blank samples, and the recovery rates of the 3 kinds of samples were 70%?114%, 72%?121%, and 70?121%. Conclusion The aTFME pretreatment applied in this study has the advantages of simple operation, high efficiency, low consumption of organic reagents, reuse, and high sensitivity, which provide technical support for the detection of pesticides in agricultural products.