超高效液相色谱--串联质谱法测定果蔬汁中甲霜灵、戊唑醇及毒死蜱

Determination of Fruit and Vegetable Juice by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry Metalaxyl,Tebuconazole and Chlorpyrifos

建立了超高效液相色谱-串联质谱法同时测定果蔬汁中甲霜灵、戊唑醇及毒死蜱残留量的分析检测方法。果蔬汁样品经1%乙酸乙腈溶液QuEChERS前处理方法,涡旋离心提取后,用液相色谱串联质谱联用仪检测分析。毒死蜱、甲霜灵及戊唑醇均采用电喷雾正离子(ESI+)电离,多反应检测模式(MRM)监测基质标准溶液外标法定量。结果表明,甲霜灵、戊唑醇及毒死蜱分别在0.1~0.5 mg/L浓度范围内线性良好,R2>0.99。在0.2 mg/kg、0.3 mg/kg和0.4 mg/kg添加水平下,甲霜灵、戊唑醇、毒死蜱的回收率分别为91.5%~106%,87.5%~89.8%和84.2%~91.7%;相对标准偏差(RSD,n=5)分别在1.7%~2.2%,0.7%~2.2%和0.9%~5.0%。本方法简捷快速,灵敏度高,重现行好,适用于果蔬汁中甲霜灵、戊唑醇和毒死蜱的快速测定。

In this study, a method for the determination of Chlorpyrifos(CPS, o,o-diethyl-o-(3,5,6-trichloro-2-pyridyl)phosphorothioate),metalaxyl(N-(2,6-dimethylphenyl)-N-(methoxy acetyl)-alanine methyl ester) and tebuconazole(1-(4-chlorophenyl)-4,4-dimethyl-3-(1 H-1,2,4-triazol-1-ylmethyl)pentan-3-ol) in fruit and vegetable juice was established by UPLC-tandem mass spectrometry. Adopted QuEChERS purification method, separated by BEH C18 ultra high performance liquid chromatography column, positived ion electrospray mode, determined by multi-reaction detection, and quantified by matrix matching standard curve. Results showed that metalaxyl, tebuconazole and CPS had a good linear relationship within the detection range of 0.5 mg/L, 0.4 mg/L, 0.3 mg/L, 0.2 mg/L and 0.1 mg/L(R^2≥0.995). The recoveries of 0.2~0.4 mg/kg were 91.5%~106%, 87.5%~89.8% and 84.2%~91.7%, respectively. The relative standard deviations were 1.7%~2.2%, 0.7%~2.2% and 0.9%~5.0%, respectively. This method is rapid, simple, efficient, and suitable for the rapid detection and quantitative determination of metalaxyl, tebuconazole and CPS in fruit and vegetable juice.