食品科学

• 分析检测 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定粮谷中6种植物生长调节剂残留

徐生坚,曹 慧,陈小珍   

  1. 浙江省质量检测科学研究院,浙江 杭州 310013
  • 出版日期:2013-09-25 发布日期:2013-09-27

Determination of Plant Growth Regulator Residues in Grains by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

XU Sheng-jian,CAO Hui,CHEN Xiao-zhen   

  1. Zhejiang Institute of Quality Inspection Science, Hangzhou 310013, China
  • Online:2013-09-25 Published:2013-09-27

摘要:

建立粮谷中多种植物生长调节剂残留量检测的超高效液相色谱-串联质谱的分析方法。样品经甲醇-水(90:10,v/v)提取,浓缩后经WAX小柱净化,采用Waters C18色谱柱分离,以乙腈和2mmol/L甲酸铵溶液为流动相进行梯度洗脱,采用电喷雾-负离子多反应监测模式,外标法定量。在5~150μg/L的质量浓度范围内,各种植物生长调节剂相关系数均大于0.9995,该方法的检出限在0.5~1.5μg/kg之间,定量限在1.5~5.0μg/kg之间。添加5.0、10.0μg/kg和25.0μg/kg三个不同水平时,6种植物生长调节剂的回收率在70.4%~119.0%之间,日内和日间相对标准偏差在1.68%~8.25%之间。该方法简单、灵敏度高、分析时间短,适用于多种植物生长调节剂的测定。

关键词: 超高效液相色谱-串联质谱, 植物生长调节剂, 残留, 粮谷

Abstract:

A method was established for determining plant growth regulator residues in grains by ultra performance liquid
chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were extracted with methanol-water (90:10, V/V), and cleaned
up on a WAX cartridge. The target analytes were separated on a Waters C18 column with gradient elution using a mobile
phase made up of acetonitrile and 2 mmol/L ammonium formate. Detection was carried out using negative electrospray
ionization and multiple reaction monitoring (MRM), and the external standard method was used for quantification. In the
linear range 5–150 μg/L, the correlation coefficient was larger than 0.9995 for each plant growth regulator. The limits of
detection (LOD) were 0.5–1.5 μg/kg, and the limits of quantitation (LOQ) were 1.5–5.0 μg/kg. The spiked recovery rates at
three levels of 5.0, 10.0 μg/kg and 25.0 μg/kg were in the range of 70.4%–119.0%. The relative standard deviation (RSD)
of intra-day and inter-day assays was 1.68%–8.25%. The method proved to be simple, sensitive, rapid and suitable for the
determination of plant growth regulator residues in grains.

Key words: ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS), plant growth regulator, residue, grains