[关键词]
[摘要]
建立了一种快速高效的分析水稻中的13种植物激素超高效液相色谱-串联质谱法。实验优化了色谱分离条件和质谱检测参数。采用ACQUITY UPLC BEH C18(2.1 mm×100 mm,i.d. 1.7 μm)分离,以甲酸-乙腈(含0.04%甲酸,V/V)和甲酸-水(含0.04%甲酸,V/V)溶液为流动相进行梯度洗脱,在11 min内基本实现了基线分离。质谱采用电喷雾离子源电离、以负离子扫描,多反应监测模式检测。结果表明,13种待测物在1~500 ng/mL质量浓度范围内线性良好,相关系数均大于0.9980;回收率为81.90%~118.80%范围内,相对标准偏差(RSD,n=3)介于2.45%~8.12%之间。该方法操作简单,灵敏度高,结果准确可靠,可用于水稻中13种植物激素含量的测定,对深入研究水稻的生长与发育过程以及鉴定植物激素残留限量等提供技术支持。
[Key word]
[Abstract]
A rapid and efficient method based on ultra-performance liquid chromatography-tandem mass spectrometry was established for the analysis of 13 plant hormones in rice. The conditions for chromatographic separation and mass spectrometry detection were optimized. The target compounds were separated by ACQUITY UPLC BEH C18 (2.1 mm × 100 mm, id 1.7 μm) with gradient elution using acetonitrile (0.04% V/V formic acid) and water (0.04% V/V formic acid) solutions as the mobile phase; baseline separation was achieved within 11 min. The 13 plant hormones were determined in the electrospray positive ionization (ESI+) and multiple reactions monitoring (MRM) modes. Analysis of the results indicated that the 13 plant hormones had good linearity in the concentration range from 1 to 500 ng/mL, and the correlation coefficients were all greater than 0.9980; the recoveries ranged between 81.9% and 118.8%, and the relative standard deviations (RSD, n=3) were between 2.45% and 8.12%. The method is simple, sensitive, accurate, and reliable; therefore, it is suitable for determining the contents of 13 kinds of plant hormones in rice. Furthermore, it can provide technical support for detailed examination of the growth and development process of rice and the identification of plant hormone residue limits.
[中图分类号]
[基金项目]
广西自然科学基金重点项目(2018GXNSFDA281024);国家自然科学基金项目(41877493);广西高校中青年教师科研基础能力提升项目(2020KY06038);广西自然科学基金青年项目(2021GXNSFBA075041);桂林理工大学科研启动基金(GUTQDJJ2020051)