超高效液相色谱-串联质谱法测定蔬菜和水果中腈吡螨酯残留量

发布时间：2018-04-28 15:42

本文选题：超高效液相色谱-串联质谱(UPLC-MS/MS) + 蔬菜　；参考：《分析测试学报》2017年01期

【摘要】：建立了蔬菜和水果中腈吡螨酯残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品经乙腈均质提取,混合使用乙二胺-N-丙基硅烷(PSA)和C18两种基质分散净化剂净化,净化液过膜后直接进行UPLC-MS/MS检测。通过考察腈吡螨酯在不同果蔬样品中的基质效应发现,采用UPLC-MS/MS检测蔬菜和水果中腈吡螨酯残留量时,腈吡螨酯在不同种类样品中存在不同程度的基质减弱效应,采用空白基质溶液稀释标准建立校正的标准曲线外标法定量以消除基质效应。结果表明,腈吡螨酯在0.05~10μg/L浓度范围内具有良好的线性关系,相关系数不低于0.999 6。在0.000 05~2 mg/kg范围内进行加标回收率实验,平均回收率为81.1%~99.3%,相对标准偏差为4.7%~9.3%,方法的定量下限为0.043μg/kg,检出限为0.013μg/kg。
[Abstract]:A high performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) method for the determination of pyrromate residues in vegetables and fruits was established. The samples were extracted by acetonitrile homogenization and purified with two kinds of matrix dispersion and purifying agent (ethylenediamine-N-propylsilane) and C18 respectively. The purified solution was directly detected by UPLC-MS/MS after the purification solution was over the membrane. By investigating the matrix effect of pyrromate in different fruit and vegetable samples, it was found that there was a different degree of matrix weakening effect of pyrromate in different kinds of samples when UPLC-MS/MS was used to detect the residual amount of pyrromate in vegetables and fruits. The corrected standard curve external standard was established by using the dilution standard of blank matrix solution to eliminate the matrix effect. The results showed that the calibration curve of pyrromate was linear in the concentration range of 0.05 渭 g / L, and the correlation coefficient was not lower than 0.999. The average recovery rate was 81.1% and 99.3%, the relative standard deviation was 4.7 渭 g / kg. The lower limit of the method was 0.043 渭 g / kg and the detection limit was 0.013 渭 g 路kg ~ (-1) 路min ~ (-1) 路min ~ (-1).
【作者单位】：山东出入境检验检疫局检验检疫技术中心;山东省农业科学院植物保护研究所;
【基金】：山东出入境检验检疫科研项目(SK201425)
【分类号】：TS255.7;O657.63

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