超高效液相色谱-串联质谱法快速检测番茄酱中吡虫啉等6种农药残留

Rapid determination of 6 pesticide residues in tomato paste by ultra performance liquid chromatography tandem mass spectrometry

建立了番茄酱中吡虫啉、多菌灵、甲基硫菌灵、霜霉威、灭多威和烯酰吗啉等农药残留的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。样品用含0.1%(体积分数)乙酸的甲醇-水(1∶1,v/v)混合溶液提取,采用Wa-ters Acquity UPLC BEH C18色谱柱,以甲醇和10 mmo l/L乙酸铵溶液为流动相进行梯度洗脱分离,经电喷雾正离子(ESI+)电离及多反应监测(MRM)模式来测定目标化合物,采用基质标准溶液曲线法进行定量。结果表明:6种农药在0.005～0.2 mg/L的范围内线性关系良好(r>0.995);当标准添加水平为0.02、0.05和0.2 mg/kg时,回收率为66.8%～102.9%;相对标准偏差均小于15%;6种农药的定量限(以信噪比(S/N)>10计)均为0.02mg/kg。该方法简便、快速、灵敏和准确,非常适合番茄酱中这6种农药残留的快速检测及定量分析。

An ultra performance liquid chromatography-tandem mass spectrometric method（UPLC-MS/MS） was established for the simultaneous determination of imidacloprid,carbendazim,thiophanate-methyl,propamocarb,methomyl and dimethomorph residues in tomato paste.The samples were extracted by methanol-water（1∶1,v/v） containing 0.1%（v/v） acetic acid.The separation was performed on a Waters Acquity UPLC system with a BEH C18 column with the gradient elution of methanol and water（containing 10 mmol/L ammonium acetate）.The six pesticides were determined in the modes of electrospray positive ionization（ESI＋） and multiple reaction monitoring（MRM）.The analytes were quantified by matrix-matched standard solution,and the calibration curves showed good linearity within the concentrations of 0.005 to 0.2 mg/L and the correlation coefficients（r） were more than 0.995.The average recoveries of the six pesticides ranged from 66.8% to 102.9% in the three spiked levels of 0.02,0.05 and 0.2 mg/kg.The relative standard deviations（RSDs） were all less than 15%.The limits of quantification（LOQ,S/N〉10） were 0.02 mg/kg for the all analytes.The results indicate that the method is easier,faster,more sensitive,and suitable for the qualitative and quantitative confirmation of the six pesticide residues from tomato paste.