蔬菜水果中有机磷农药的基质效应分析及检测方法选择

Matrix effects analysis and determination method selection of organophosphrous pesticides in vegetables and fruits

中文关键词:  蔬菜水果  有机磷农药  基质效应  气相色谱-串联质谱法  超高效液相色谱-串联质谱法

英文关键词:vegetables and fruits  organophosphrous pesticides  matrix effects  gas chromatography tandem mass spectrometry  ultra performance liquid chromatography tandem mass spectrometry

中文摘要:

      目的 通过对常见蔬菜水果中有机磷农药的基质效应进行全面的分析, 探索更加高效的有机磷农药残留检测手段。方法 30种(11类)供试蔬果样品分别利用乙腈提取, 经QuEChERS净化后, 配制溶剂标准工作曲线和基质标准工作曲线, 利用气相色谱-串联质谱法(gas chromatography tandem mass spectrometry, GC-MS/MS)和超高效液相色谱-串联质谱法(ultra performance liquid chromatography tandem mass spectrometry, UPLC-MS/MS)分析19种有机磷农药的基质效应表现。结果 利用GC-MS/MS分析得到的19种有机磷农药的溶剂标准曲线及其30种基质标准曲线在10~200 μg/L浓度范围内线性关系良好, 利用UPLC-MS/MS分析得到的19种有机磷农药的溶剂标准曲线及其30套基质标准曲线在4~100 μg/L浓度范围内线性关系良好, 所有工作曲线的线性相关系数(r2)均大于0.99; 利用GC-MS/MS分析时, 大部分供试农药在供试基质中呈较强的基质增强效应, 其中水胺硫磷的基质效应最强, 西葫芦可以有效校正供试农药的基质效应; 利用UPLC-MS/MS分析时, 供试农药以弱基质效应表现为主, 西葫芦对供试农药基质效应的校正能力不明显。结论 在利用GC-MS/MS检测供试有机磷农药时, 可用西葫芦配制基质匹配标准溶液进行定量分析; 在利用UPLC-MS/MS检测供试有机磷农药时, 除了乙酰甲胺磷、乐果、敌敌畏、亚胺硫磷, 其他农药均可利用溶剂标准溶液进行定量分析。

英文摘要:

      Objective To analyze the matrix effect of organophosphorus pesticides in common vegetables and fruits, and explore a more efficient detection method of organophosphorus pesticide residues. Methods The samples of tested vegetables and fruits (30 kinds including 11 different types) were extracted by acetonitrile and purified by QuEChERS methods, then the solvent calibration curves and matrix matched calibration curves were prepared. The matrix effects of 19 organophosphrous pesticides were analyzed by gas chromatography tandem mass spectrometry (GC-MS/MS) and ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Results The solvent calibration curves of 19 organophosphrous pesticides and 30 matrix matched calibration curves showed an excellent linearity in the range of 10?200 μg/L (GC-MS/MS) and 4?100 μg/L (UPLC-MS/MS), and the determination coefficients (r2) were more than 0.99. Most tested pesticides showed strong matrix effects, isocarbophos exhibited the strongest matrix enhancement effects and zucchini could effectively compensate the matrix effects when GC-MS/MS method was used. Most tested pesticides performed weak matrix effects, the compensation of matrix effects didn’t get a better result by zucchini when UPLC-MS/MS method was used. Conclusion When using GC-MS/MS to detect test organophosphorus pesticides, a standard solution of matrix matching can be prepared from zucchini for quantitative analysis. When using UPLC-MS/MS to detect test organophosphorus pesticides, except for acephate, dimethoate, dichlorvos, imidophos, other pesticides can be quantitatively analyzed using solvent standard solutions.