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应用液相色谱-电喷雾电离三级四极杆串联质谱(LC-ESI-MS/MS)仪器,建立测定棉花中7种烟碱类农药残留的检测方法。样品先添加同位素内标吡虫啉-D4,再用乙腈超声提取、浓缩,乙腈-甲酸(0.15%)溶液溶解,以ZORBAX Eclipse XDB-C8色谱柱为分离柱。液相色谱-串联质谱仪采用正离子扫描方式,多反应监测,每种烟碱类农药各选2对离子进行定性、定量分析,除吡虫啉外均采用外标法定量。在0~12.5μg/L测定范围内此方法具有良好的线性关系(r>0.99),在10、20和40μg/kg 3个水平进行添加回收实验,平均回收率范围为75.9%~98.4%;相对标准偏差小于15.8%;方法检测低限(LOQ)均为10μg/kg。
A liquid chromatography-electrospray ionization triple quadrupole mass spectrometry (LC-ESI-MS / MS) instrument was established to determine the detection method of seven nicotine pesticide residues in cotton. Samples were first added isotope internal standard imidacloprid-D4, then extracted with acetonitrile, concentrated, acetonitrile-formic acid (0.15%) solution was dissolved to ZORBAX Eclipse XDB-C8 column as the separation column. Liquid chromatography - tandem mass spectrometry using positive ion scanning mode, multi-reaction monitoring, each of two nicotinic pesticides selected two qualitative and quantitative analysis of ions, except for imidacloprid external standard method were used. The method had a good linear relationship (r> 0.99) within the range of 0 ~ 12.5μg / L, and the average recoveries ranged from 75.9% to 98.4% at the recoveries of 10, 20 and 40μg / kg. The relative standard deviation was less than 15.8%. The LOQ was 10μg / kg.