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.
journal_name
Food Chemjournal_title
Food chemistryauthors
Dong X,Liang S,Shi Z,Sun Hdoi
10.1016/j.foodchem.2015.07.025subject
Has Abstractpub_date
2016-02-01 00:00:00pages
432-40eissn
0308-8146issn
1873-7072pii
S0308-8146(15)01030-4journal_volume
192pub_type
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