热带水果中5种农药残留UPLC-MS/MS测定的基质效应研究

赵婧 何燕 钱兵 张月 韩丙军 彭黎旭

摘  要：研究了超高效液相色譜-串联质谱法（UPLC-MS/MS）检测噻唑磷、戊唑醇、螺虫乙酯、嘧菌酯和氯虫苯甲酰胺5种农药残留时，香蕉、芒果、菠萝和哈密瓜4种热带水果样品对其残留测定的基质效应。结果表明，5种农药在0.005～0.5 μg/mL浓度范围内，线性关系良好，相关系数优于0.999，加标回收率为76%～130%，相对标准偏差为0.2%～ 12.9%（n=5）。4种热带水果基质中，噻唑磷、螺虫乙酯、嘧菌酯和氯虫苯甲酰胺普遍呈基质增强效应，为97.0%～178.8%;戊唑醇在低浓度时呈基质抑制效应，为56.6%～65.7%，其余为基质增强效应。4种热带水果中，芒果的基质效应较为明显，为63.0%～178.8%;5种农药中，戊唑醇和螺虫乙酯的基质效应较为明显，戊唑醇为56.6%～129.9%，螺虫乙酯为107.1%～178.8%。在日常检测工作中，建议采用基质匹配标准曲线进行定量分析，以提高检测结果的准确性。研究结果可为热带水果中农药残留的检测提供依据，并为减小基质效应提供参考。

关键词：基质效应;超高效液相色谱-串联质谱法;热带水果;农药残留

中图分类号：TS255.7      文献标识码：A

Matrix Effects in the Determination of 5 Pesticides in Tropical Fruits by UPLC-MS/MS

ZHAO Jing1，2， HE Yan2， QIAN Bing2，3， ZHANG Yue2， HAN Bingjun2*， PENG Lixu4

1. College of Plant Protection， Hainan University， Haikou， Hainan 570228， China; 2. Analysis & Testing Center， Chinese Academy of Tropical Agricultural Sciences / Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables， Haikou， Hainan 571101， China; 3. College of Forestry， Hainan University， Haikou， Hainan 570228， China; 4. Environment and Plant Protection Institute， Chinese Academy of Tropical Agricultural Sciences， Haikou， Hainan 571101， China

Abstract： The matrix effect of banana， mango， pineapple and muskmelon on the determination of fosthiazate， tebuconazole， spirotetramat， azoxystrobin and chlorantraniliprole residues in four tropical fruits was studied by UPLC- MS/MS. The results showed that in the range from 0.005 to 0.5 μg/mL， the coefficient of determination （r） was greater than 0.999. The recovery （n=5） was 76%-130% with relative standard deviations （RSDs） of 0.2%-12.9%. Fosthiazate， spirotetramat， azoxystrobin and chlorantraniliprole showed matrix enhancing effect in four tropical fruit matrixes， ranging from 97.0% to 178.8%. Tebuconazole at low concentration showed matrix inhibitory effect， ranging from 56.6% to 65.7%， the rest showed matrix enhancing effect. Among them， the matrix effect of mango in the four tropical fruits was more obvious， which was 63.0%-178.8%. Tebuconazole and spirotetramat in the five pesticides were more obvious， tebuconazole was 56.6%-129.9%， spirotetramat was 107.1%-178.8%. In actual detection， it is recommended to use matrix-matched standards for quantitative analysis for enhancing the accuracy of testing results. This experiment could provide a basis for the detection of pesticide residues in tropical fruits， and provide a reference for the reduction of matrix effect.

Keywords： matrix effects; ultra performance liquid chromatography-tandem mass spectrometry; tropical fruits; pesticide residue

DOI： 10.3969/j.issn.1000-2561.2021.06.034

热带水果作为我国的重要经济作物，其种类繁多，营养丰富，品质优良，近年来随着种植面积和产量逐渐增大，相关产业已占据国民经济的重要地位。热带地区病虫害发生日益严重，农药使用量也逐年增加，而农药残留超标不仅对食品安全造成一定影响，也会导致人类健康和环境受到威胁[1-3]。因此，亟需对热带水果中的农药残留进行准确的测定，以保证我国热带水果的安全生产。

目前，用于农药残留的检测方法主要是液相色谱-质谱检测法（LC-MS/MS）[4-8]，其对基质复杂、干扰严重的痕量化合物能进行很好地定性定量，现已广泛应用于医药、食品安全等领域。……