超高效液相色谱-四级杆/静电场轨道阱高分辨质谱测定豆芽中的11种植物生长调节剂

Determination of 11 plant growth regulator in bean sprouts by UPLC-Q-Orbitrap HRMS

建立了超高效液相色谱-四级杆/静电场轨道阱高分辨质谱测定豆芽中11种植物生长调节剂的检测分析方法。样品基于QuEChERS技术,以10 mL含1%甲酸的乙腈提取,C18净化,0.1%甲酸5 mmol/L乙酸铵水溶液梯度洗脱,RRHD SB-Aq色谱柱分离,在电喷雾离子源(ESI)、全扫描/数据依赖二级质谱扫描(Full MS/dd-MS^2)监测模式下正负切换同时进行检测。结果表明,11种化合物线性关系良好(相关系数噻苯隆R^2=0.992,其余R^2>0.998),定量限为(0.3～3)μg/kg;平均加标回收率为84.6%～113.1%,相对标准偏差为0.6%～8.3%。该方法简单快速、灵敏度高、结果准确,可对豆芽中11种植物生长调节剂进行有效的快速筛查和定量分析。

A QuEChERS method was developed for the simultaneous detection of 11 plant growth regulator residues in bean sprouts by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q-Orbitrap HRMS). The samples were extracted with acetonitrile containing 1%(v/v) formic acid and purified with C18, gradient elution with 0.1% formate ammonium acetate(5 mmol/L). The separation of the 11 plant growth regulators was performed on RRHD SB-Aq column with gradient elution. The compounds were detected by positive and negative ion of Full scan/date dependent MS/MS(Full MS/dd-MS2) via electron spray ionization(ESI) source. The result showed that the calibration curves of 11 plant growth regulator were linear with correlation coefficients(R^2)greater than 0.998(TDZ=0.992), the limits of detection(LODs) ranged from 0.3 μg/kg to 3 μg/kg and the average recoveries were between 84.6% to 113.1% with relative standard deviations(RSDs) from 0.6% to 8.3%. The method established in this paper is simple, accurate and sensitive. This method can be used for the rapid screening and quantitative analysis of 11 plant growth regulator residues in bean sprouts.