改良QuEChERS结合超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定果蔬中15种植物生长调节剂残留

Determination of 15 Plant Growth Regulators Residues in Fruits and Vegetables by Modified QuEChERS Coupled with UPLC-Q-Orbitrap HRMS

基于改良的QuEChERS方法,建立超高效液相色谱-四级杆/静电场轨道阱高分辨质谱法(UPLC-Q-Orbitrap HRMS)快速筛查和测定果蔬中15种植物生长调节剂残留的方法。样品以1%乙酸乙腈提取,多壁碳纳米管(MWCNTs)净化,采用Hypersil GOLD aq C18色谱柱(2.1 mm×100 mm,1.9μm)进行分离,乙腈和水(含0.1%甲酸-5 mmol/L甲酸铵)为流动相梯度洗脱,质谱采用全扫描/数据依赖的二级扫描模式,基质匹配校准曲线定量。结果显示:15种化合物在2.0~500.0μg/L范围内,线性关系良好(r>0.990);在3个加标水平下,平均回收率为70.3%~107.2%,相对标准偏差(RSD)为1.4%~9.9%,定量限为10.0~20.0μg/kg。该方法简单,灵敏度高,准确可靠,可对果蔬中植物生长调节剂进行快速筛查和定量分析。

A method was developed for the simultaneous determination of 15 plant growth regulators residues in fruits and vegetables by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q-Orbitrap HRMS)with modified QuEChERS. The samples were extracted by acetonitrile containing 1% acetic acid and purified by MWCNTs,separated on a Hypersil GOLD aq C18 column(2.1 mm×100 mm,1.9 μm),gradient elution with acetonitrile and water(containing 0.1% formic acid-5 mmol/L ammonium formate). The target compounds were analyzed in full scan/data-dependent MS2(Full MS/dd-MS2)mode,and quantified by using the matrix-matched standard calibration. The results showed that the correlation coefficients was over than 0.990 in the range of 2.0~500.0 μg/mL.The three-level spiked recoveries were between from 70.3% to 107.2% with relative standard deviation from 1.4% to 9.9%. The limits of quantitation were 10.0~20.0 μg/kg. The method was simple,sensitive,accurate and suitable for the rapid screening and quantitative analysis of plant growth regulators in fruits and vegetables.