番茄中复硝酚钠、胺鲜酯残留量的分析检测

Analysis and detection of residual sodium nitrophenolate and diethyl aminoethyl hexanoate in tomato

[目的]采用超高效液相色谱-串联质谱(UPLC-APCI-MS/MS)对复硝酚钠(邻硝基苯酚钠、对硝基苯酚钠、5-硝基愈创木酚钠)和胺鲜酯在番茄中的检测方法进行优化,创建完整分析方法。[方法]样品需经乙腈提取,经MgSO4、PSA、GC-e制备的吸附剂组合物进行净化后,UPLC-APCI-MS/MS方法检测。[结果]在0.05~2.0 mg/L质量浓度范围内,邻硝基苯酚钠的质量浓度与其峰面积线性关系基本保持良好,R^(2)值为0.9995;0.01~0.20 mg/L质量浓度范围内,其他3种化合物R^(2)值均≥0.99;邻硝基苯酚钠在番茄中0.05(LOQ)、0.25、0.50 mg/kg 3个标准添加质量分数水平,其平均回收率在81%~99%之间,相对标准偏差在0.6%~7.3%之间,其他3种化合物在0.01(LOQ)、0.05、0.10 mg/kg 3个标准添加质量分数水平下,平均回收率在92%~113%之间,相对标准偏差在1.2%~9.1%之间。运用该检测方法对采自吉林、山西、宁夏、北京、河北、河南、山东、安徽、浙江、湖南、贵州、云南共12个区域的番茄样品进行采样检测,结果显示,所有田间样品中上述4种农药的化学残留量均未超出中国规定的最大残留限量标准(MRLs),并通过储藏稳定性试验证实检测结果有效。[结论]此检测分析筛选方法对样品具有较好的提取、分离效果、操作分离过程更加简便与高效、灵敏度较高和样品通用性强等多项优点,适用于对番茄品种中的4种农药筛查及其残留含量的同时检测。

[Aims]To establish a complete analytical method for the determination of sodium nitrophenolate(sodium o-nitrophenolate,sodium p-nitrophenolate,sodium 2-methoxy-5-nitrophenolate)and diethyl aminoethyl hexanoate in tomato,which were optimized by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-APCI-MS/MS).[Methods]The samples were extracted by acetonitrile,purified by the adsorbent compositions prepared by MgSO4,PSA and GC-e,and then detected by UPLC-APCI-MS/MS method.[Results]In the range of0.05-2.0 mg/L,the linear relationship between the mass concentration of sodium o-nitrophenol and the measured peak area was basically good,and the R^(2)value was 0.9995.In the range of 0.01-0.20 mg/L,the R^(2)values of the other 3 compounds were all≥0.99.At 0.05(LOQ),0.25 and 0.50 mg/kg,the average recoveries of sodium o-nitrophenol in tomato were between 81%and 99%,and the relative standard deviations were between 0.6%and 7.3%.The average recoveries of the other 3 compounds ranged from 92%to 113%and the relative standard deviations ranged from 1.2%to 9.1%at 0.01(LOQ),0.05 and 0.10 mg/kg.The tomato samples collected from Jilin,Shanxi,Ningxia,Beijing,Hebei,Henan,Shandong,Anhui,Zhejiang,Hunan,Guizhou and Yunnan were tested by this detection method.The results showed that the chemical residues of the above 4 pesticides in all the field samples did not exceed the maximum residue limits(MRLs)stipulated by China.The results were validated by storage stability test.[Conclusions]The detection,analysis and screening method has many advantages,such as good separation and purification effect,more simple and efficient separation process,high sensitivity and wide sample usability,which is suitable for the screening of the 4 pesticides in tomato and the simultaneous detection of their residual content.