高效液相色谱串联质谱法测定水果、蔬菜中双胍辛胺的定性定量分析研究

Determination of Iminoctadine in Fruits and Vegetables by High Performance Liquid Chromatography-Tandem Mass Spectrometry

目的:建立水果和蔬菜中双胍辛胺的高效液相色谱串联质谱法的定性定量分析方法。方法:样品经过正丁醇∶正己烷=1∶1混合溶液提取,再用酸化水净化。以高效液相色谱质谱联用仪检测萃取液中的双胍辛胺的含量,采用HILIC-C18柱分离,在ESI正离子模式下,以质谱多反应监测,采用外标法进行定量分析。结果:在10~500 ng·mL^(-1),双胍辛胺的线性良好,相关系数R> 0.995,检出限为0.002 0 mg·kg^(-1),定量限为0.011 mg·kg^(-1),双胍辛胺在3个浓度添加水平下,水果回收率在92.7%~108.9%,蔬菜回收率在96.2%~110.0%,水果相对标准偏差为1.15%~4.45%,蔬菜相对标准偏差为1.36%~2.15%。结论:本研究建立的高效液相色谱串联质谱法测定双胍辛胺的方法准确、快速,能够满足水果、蔬菜中双胍辛胺的分析要求。

Objective: A method was developed for the determination of iminoctadine of fruits and vegetables by high performance liquid chromatography-tandem mass spectrometry. Method: The sample was extracted with the solution of butyl alcohol and hexane(1 ∶ 1), and then cleaned-up by acidified water. Iminoctadine was determined by liquid chromatography mass spectrometer with a HILIC chromatographic column, analyzed in positive electronic spayionization(ESI+) mode with multiple reaction monitoring, and quantified by the external standart method. Result: The calibration curves were linear with the correlation coefficients over 0.995 in the range of 10 ~ 500 ng·mL^(-1) for iminoctadine.The limits of detection were 0.002 0 mg·kg^(-1). The limits of quantification were 0.011 mg·kg^(-1). The mean recoveries of iminoctadine at three spiked levels were in the range from 92.7% to 108.9% of fruits and 96.2% ~ 110.0% of vegetables,with the relative standard deviations were in the range from 1.15% ~ 4.45% of fruits and 1.36% ~ 2.15% of vegetables.Conclusion: Determination of iminoctadine in fruits and vegetables by high performance liquid chromatography-tandem mass spectrometry was established in this study which was accurate and rapid, suitable for analysis of iminoctadine in fruits and vegetables.