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目的建立超高效液相色谱-串联质谱方法同时测定水果中多效唑、赤霉素、噻苯隆等6种植物生长调节剂和甲基硫菌灵、甲霜灵、烯酰吗啉等8种杀菌剂残留。方法样品经含1%乙酸的乙腈溶液提取,无水硫酸镁-醋酸钠盐析,分散固相萃取吸附剂(C18粉末和无水硫酸镁)净化,采用ZORBAX XDB C18色谱柱(100 mm×2.1 mm,1.8μm)进行分离,流动相为乙腈-0.1%甲酸+10 mmol/L乙酸铵水,梯度洗脱,电喷雾正离子和负离子模式进行质谱测定。结果 8种杀菌剂和6种植物生长调节剂在2.0~100.0 ng/m L范围线性关系均良好,相关系数(r)>0.999 0;方法的检出限为0.5~3.0μg/kg,定量限为1.5~9.0μg/kg;空白样品的加标浓度为10.0、50.0和100.0μg/kg时,回收率为79.5%~93.0%,相对标准偏差为2.1%~8.7%。结论该方法适用于同时检测水果中8种杀菌剂和6种植物生长调节剂残留。
OBJECTIVE To establish a method for the simultaneous determination of 6 plant growth regulators and thiophanate-methyl, metalaxyl and dimethomorph in fruits by ultra performance liquid chromatography-tandem mass spectrometry Residues. Methods The samples were extracted with 1% acetic acid in acetonitrile, purified by anhydrous magnesium sulfate-sodium acetate, dispersed solid-phase extraction adsorbents (C18 powder and anhydrous magnesium sulfate) and analyzed by ZORBAX XDB C18 column (100 mm × 2.1 mm, 1.8μm). The mobile phase was acetonitrile-0.1% formic acid + 10 mmol / L ammonium acetate, gradient elution, electrospray positive ion and negative ion mode. Results The linear relationship between 8 kinds of fungicides and 6 kinds of plant growth regulators in the range of 2.0-100.0 ng / m L was good with the correlation coefficient (r)> 0.999 0. The detection limit was 0.5-3.0 μg / kg, and the limit of quantification And the recoveries were 79.5% ~ 93.0% and the relative standard deviations were 2.1% ~ 8.7% at spiked concentrations of 10.0, 50.0 and 100.0 μg / kg respectively. Conclusion The method is suitable for simultaneous determination of 8 fungicides and 6 plant growth regulators residues in fruits.