GPC/SPE-UPLC-MS/MS凝胶色谱仪辅助分散型固相萃取-快速检测桃胶中10种杀虫剂和杀菌剂农药残留

GPC/SPE-UPLC-MS/MS-rapid determination from GPC and dispersed solid phase extraction of 10 insecticides and fungicides residues in peach gum

建立了桃胶中啶虫脒、吡虫啉、辛硫磷等10种杀虫剂和杀菌剂农药的超高效液相色谱-串联质谱法(Ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)快速筛查方法。样品以有机溶剂乙腈作为萃取试剂,以分散型固相萃取净化,必要时以凝胶色谱(GPC)辅助净化,经Zorbax Eclipse Plus C18(2.1 mm×50 mm,1.8μm)反相色谱柱分离,以甲醇-水溶液(含0.1%甲酸和5 mmol/L乙酸铵)为流动相,梯度洗脱,以LC-MS/MS分析,外标法基质配标定量。10种杀虫剂和杀菌剂农药在1.0 ng/mL~40.0 ng/mL浓度范围内线性良好,r^(2)≥0.997,定量限为0.005 mg/kg,高于现有桃胶检测相关文献研究水平。在0.005,0.010,0.050 mg/kg这3组添加水平下,目标物的平均回收率为80.0%~105.4%,相对标准偏差(RSD)为0.6%~3.2%。该方法前处理操作简便,定性定量准确,适用于桃胶中10种杀虫剂和杀菌剂农药残留的检测。

A rapid screening method for 10 insecticides and fungicides in peach gum by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.The samples were separated by Zorbax Eclipse Plus C18(2.1 mm×50 mm,1.8μm)reversephase chromatographic column.Methanol-aqueous solution(containing 0.1%formic acid and 5 mmoL/L ammonium acetate)was used as the mobile phase.Gradient elution was performed,analyzed by LC-MS/MS,and quantified by external standard method.The 10 insecticides and fungicides had good linearity in the concentration range of 1.0 ng/mL to 40.0 ng/mL,r^(2)≥0.997,and the limit of quantification was 0.005 mg/kg,which was higher than the level of the existing literature on peach gum detection.At the supplemental levels of 0.005,0.010 and 0.050 mg/kg,the average recoveries of the target compounds were 80.0%to 105.4%,and the relative standard deviations(RSD)were 0.6%to 3.2%.The method is simple,rapid,qualitative and quantitative,which is suitable for the detection of 10 kinds of insecticides and fungicides in peach gum.