Fan Zhichen, Han Zheng, Guo Wenbo, Zhao Zhihui
College of Food Science & Technology, Shanghai Ocean University, Shanghai 201306, China.
Institute for Agro- Food Standards and Testing Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China.
Se Pu. 2017 Jun 8;35(6):627-633. doi: 10.3724/SP.J.1123.2017.02010.
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% (=5). Good linear relationships were obtained, the correlation coefficients () were greater than 0.99. The limits of detection (LODs, =3) and the limits of quantification (LOQs, =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.
建立了一种使用QuEChERS预处理程序结合超高效液相色谱-串联质谱法（UHPLC-MS/MS）同时测定不同饲料产品中30种霉菌毒素的方法。样品用5 mL水和5 mL含1%（v/v）甲酸的乙腈提取。取一部分上清液用氮气吹干，再用1 mL含5 mmol/L醋酸铵-乙腈（80:20，v/v）的水溶液复溶，然后用UHPLC-MS/MS分析。采用基质匹配校准曲线和内标进行准确定量。在低、中、高加标水平下，回收率令人满意，范围为72.0%至118.4%（n = 5）。获得了良好的线性关系，相关系数（r）大于0.99。检测限（LODs，n = 3）和定量限（LOQs，n = 10）分别为0.7 μg/L至20 μg/L和2 μg/L至50 μg/L。所提出的方法简单、快速且有价值，可成为预混料、浓缩饲料和配合饲料产品中30种霉菌毒素定量分析的有力工具。
