QuEChERS结合GC-MS/MS测定41种农残及方法耐用性探究

QuEChERS前处理方法结合气相色谱串联质谱(GC-MS/MS)检测是目前果蔬中多农残分析的主流方法。QuEChERS方法净化效果对GC-MS/MS检测结果影响显著,特别是净化管中石墨化碳黑(GCB)的含量,对上述多农残检测方法耐用性至关重要。本文选取甘薯叶、辣椒、甘蓝以及葡萄作为试验对象,通过研究不同GCB含量的Qu ECh ERS方法,以GC-MS/MS检测41种农药的添加回收率、精密度和方法耐用性等指标。结果表明,GCB含量为15 mg时平均回收率总体在65%~110%(除百菌清和五氯硝基苯),相对标准偏差(RSD)在12%以下,在浓度0.005~0.5 mg·L^-1范围内方法线性良好,连续进样200针时,质控样各检测参数响应变化在±30%以内。证明该法适用于大批量样品前处理及GC-MS/MS分析,方法精密度、准确度、耐用性等指标表现良好。

Determination of 41 Pesticide Residues by QuEChERS Combined with GC-MS/MS and Exploration of Method Durability

The QuEChERS pretreatment method combined with GC-MS/MS detection is currently the mainstream method for the analysis of multiple pesticide residues in fruits and vegetables.The purification effect of QuEChERS method has a significant impact on the detection results of GC-MS/MS,especially the content of graphitized carbon black in the purification tube,which is very important to the durability of the above-mentioned multi-pesticide detection method.In this paper,sweet potato leaves,peppers,cabbage and grapes are selected as the test objects.By studying the QuEChERS method with different GCB content,the recovery rate,precision and method durability of 41 pesticides were detected by GC-MS/MS.The results show that when the GCB content is 15 mg,the average recovery rate is generally 65%~110%(except chlorothalonil and quintozene),the RSD is below 12%,and the concentration is within the range of 0.005~0.5 mg·L^-1.The linearity is good.When 200 needles are continuously injected,the response change of each detection parameter of the quality control sample is within±30%.It is proved that the method is suitable for the pretreatment of large quantities of samples and GC-MS/MS analysis,and the method has good performance in precision,accuracy,durability and other indicators.