Method for Determination of Niclosamide-Olamine Residues in Grains
A method was established to determine residue of niclosamide-olamine in grains by LC-MS/MS.Using the improved QuEChERS method,the samples were ultrasonically extracted by a certain volume ratio of ammonia acetonitrile,centrifuged at high speed in a refrigerated state,purified with PSA.They were separated by Agilent Zorbax C18 chromatographic column,detected by high-performance liquid chromatography tandem mass spectrometer,and accurately quantified by external standard method.In the concentration range of 0.2-20.0 μg/L,the concentration points of the 7 blank matrix standard curves had a good linear relationship,with the correlation coefficient(R²)＞0.995,and the detection limit of niclosamide-olamine was 0.3 μg/kg and the limit of quantification was 1.0 μg/kg.The average recoveries of six parallel tests of niclosamide-olamine in grains were 83.5%-122.7%,and the relative standard deviations were 1.1%-9.4%under three different concentration spike levels of 1.0 μg/kg,5.0 μg/kg and 10.0 μg/kg.This method has simple sample pre-treatment,short analysis time,low cost of detection consumables,and good reproducibility.It can meet the detection requirements for the residues of niclosamide-olamine in grains.
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