QuEChERS-超高效液相色谱法检测瓜果中14种植物生长调节剂残留量

Simultaneous determination of 14 plant growth regulator residues in melons and fruits by QuEChERS-ultra-high performance liquid chromatography

目的建立QuEChERS-超高效液相色谱法同时检测黄瓜、番茄等瓜果中14种植物生长调节剂残留量。方法样品经含0.5%甲酸的乙腈-二氯甲烷(1∶1,V/V)提取、分散固相萃取法净化,采用Agilent InfinityLab Poroshell 120 EC-C_(18)色谱柱(4.6 mm×100 mm, 2.7μm),0.05%乙酸和乙腈为流动相梯度洗脱,在220、254 nm同时进行检测。结果 14种植物生长调节剂在12 min内实现快速分离,在线性范围内的相关系数(r)均大于0.999,检出限为0.005～0.076 mg/kg,定量限为0.02～0.32 mg/kg,加标回收率为71.9%～113.8%,相对标准偏差(RSD)均小于5.0%。结论该方法能同时快速检测多种植物生长调节剂。操作简单,具有较好的灵敏度、精密度及回收率,检测成本低,适用于大批量样品的定量筛查。

Objective A method for the simultaneous determination of 14 plant growth regulator residues in cucumbers and tomatoes, etc. by QuEChERS-ultra-high performance liquid chromatography(UPLC) was developed. Methods The samples were extracted by CH2Cl2-CH3CN(1∶1,V/V) containing 0.5% formic acid, and purified with dispersive solid phase extraction. Chromatographic analysis was carried out on Agilent InfinityLab Poroshell 120 EC-C18 column(4.6 mm×100 mm, 2.7 μm) with acetonitrile-0.05% acetic acid as the mobile phase using gradient elution, and detected at 220 and 254 nm. Results Rapid separation of 14 analytes could be performed in 12 minutes. The correlation coefficients of calibration curves were above 0.999. The limits of detection and quantification were in the ranges of 0.005-0.076 mg/kg and 0.02-0.32 mg/kg. The average recoveries varied from 71.9% to 113.8% with relative standard deviations less than 5.0%. Conclusion The method was rapid for simultaneous determination of varied residues. It was simple,reliable and cost-effective and was suitable for quantitative screening of large quantities of samples.