采用QuEChERS前处理技术,建立了超高效液相色谱-串联质谱(UHPLC-MS/MS)检测不同饲料样品(预混料、浓缩料和配合料)中30种真菌毒素含量的分析方法.饲料样品经5 mL水和5 mL含1%(v/v)甲酸的乙腈溶液提取后,取上清液氮吹至近干,残渣经1 mL 5 mmol/L醋酸铵水溶液-乙腈(80:20,v/v)复溶后,上机测定.采用基质匹配标准曲线结合同位素内标法进行定量分析.在低、中、高3个添加水平下,30种真菌毒素的平均加标回收率为72.0%~118.4%(n=5),30种真菌毒素在各自的线性范围内线性关系良好,相关系数(r2)≥0.99,检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.7~20 μg/L和2~50 μg/L.该法简单、快速、实用性强,适用于预混料、浓缩料和配合料中30种真菌毒素的定量分析.
A method for the simultaneous determination of 30 mycotoxins in different feed products was developed using a QuEChERS pretreatment procedure coupled with ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS).The samples were extracted with 5 mL water and 5 mL acetonitrile containing 1% (v/v) formic acid.An aliquot of the supernatant was dried by nitrogen gas,re-dissolved by 1mL water containing 5 mmol/L ammonium acetate-acetonitrile (80:20,v/v),and analyzed by UHPLC-MS/MS.Matrix-matched calibration curves and internal standards were used for accurate quantification.Satisfactory recoveries at low,medium and high spiked levels were ranged from 72.0% to 118.4% (n=5).Good linear relationships were obtained,the correlation coefficients (r2) were greater than 0.99.The limits of detection (LODs,S/N=3) and the limits of quantification (LOQs,S/N=10) ranged from 0.7 μg/L to 20 μg/L and from 2 μg/L to 50 μg/L,respectively.The proposed method is simple,rapid and valuable,which can be a powerful tool for quantitative analysis of the 30 mycotoxins in premixed feed,concentrated feed and formula feed products.
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