title: Development of multi-residue analysis of herbicides in cereal grain by ultra-performance liquid chromatography-electrospray ionization-mass spectrometry.
abstract: A rapid and sensitive method was developed for the determination of 50 herbicides in cereal grain by ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS). Using acetonitrile effectively extracted 22 kinds of triazine and other basic herbicides, and using 90:10 v/v acetonitrile-phosphate buffer (pH = 7.5) effectively extracted other 28 herbicides. Chromatographic separation was achieved using gradient elution with acetonitrile-water as a mobile phase for 22 triazine and phenylurea herbicides and with 5mM ammonium acetate aqueous solution containing 0.1% formic acid-acetonitrile as a mobile phase for other 28 herbicides. Using matrix-matched standard calibration curve effectively reduced the indirect matrix effects, ensured accurate quantification for these herbicides. The response was linear over two orders of magnitude with a correlation coefficients (r(2)) higher than 0.992. The limits of quantification for the herbicides varied from 0.2 to 25.6 μg kg(-1). The intra- and inter-day precisions (relative standard deviation, RSD) were 2.2-9.3% and 5.7-17.1%, respectively. The recovery varied from 61.6% to 110% with the RSD of 1.6-11.8%. Analyzing soybean, corn and wheat samples from 17 counties evaluated this method. The developed and validated method has high sensitivity, satisfactory recovery and precision, can ensure the multi-class multi-residue analysis at low μg kg(-1) level for the most herbicides in cereal grain.
authors: College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Baoding 071002, China; Shijiazhuang Center for Disease Control and Prevention of Hebei Province, Shijiazhuang 050000, China.
authors: Xinfeng
authors: X
authors: Dong
authors: College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Baoding 071002, China.
authors: Shuxuan
authors: S
authors: Liang
authors: College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Baoding 071002, China.
authors: Zhihong
authors: Z
authors: Shi
authors: College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Baoding 071002, China. Electronic address: hanwen@hbu.edu.cn.
authors: Hanwen
authors: H
authors: Sun
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D002523:Edible Grain / Q000737:chemistry*; D006540:Herbicides / Q000032:analysis / Q000737:chemistry*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D006540:Herbicides
keywords: Cereal grain; Herbicide residues; Mass spectrometry; Ultra performance liquid chromatography