Zhou Jian, Xu Jiao-Jiao, Cong Jin-Mi, Cai Zeng-Xuan, Zhang Jing-Shun, Wang Jun-Lin, Ren Yi-Ping
Lab of Physicochemical Research, Department of Physicochemical & Toxicology, Zhejiang Provincial Center for Disease Control and Prevention, Zhejiang 310051, China; Zhejiang Provincial Key Lab of Health Risk Appraisal for Trace Toxic Chemicals, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China.
Lab of Physicochemical Research, Department of Physicochemical & Toxicology, Zhejiang Provincial Center for Disease Control and Prevention, Zhejiang 310051, China.
J Chromatogr A. 2018 Jan 12;1532:20-29. doi: 10.1016/j.chroma.2017.11.050. Epub 2017 Nov 23.
A multiclass method was proposed for the simultaneous determination of various classes of veterinary drugs (n = 65), mycotoxins and metabolites (n = 39) in egg and milk by ultra-high performance liquid chromatography-tandem mass spectrometry. The contaminants were extracted by QuEChERS-based strategy including salt-out partitioning and dispersive solid-phase extraction for cleanup further. With the aim of maximizing throughput and extraction efficiency, Plackett-Burman design was employed initially for screening significant variables. And response surface methodology based on central composite design was conducted to achieve optimal conditions in details: 3.35% (v/v) of formic acid in acetonitrile, 1.2 g of NaCl, 0.5 g of anhydrous NaAc, 300 mg of C18 and 140 mg of primary secondary amine. Satisfactory analytical characteristics in validation, in aspects of accuracy (70%-105% for mycotoxins and quinolones, 55%-80% for sulphonamides and 40%-105% for other veterinary drugs), precision (inter-day RSDs < 14%) and sensitivity (LOQs ranged from 0.01 μg/kg to 31 μg/kg), were achieved under the optimized conditions. The matrix effects were evaluated and compensated by the use of matrix-matched calibration curves (R > 0.987). In practice, 45 eggs and 30 milk samples were investigated by the established method, of which positive finding aflatoxin in milk and sterigmatocystin in eggs.
提出了一种多类方法,通过超高效液相色谱-串联质谱法同时测定鸡蛋和牛奶中的各类兽药(n = 65)、霉菌毒素和代谢物(n = 39)。采用基于QuEChERS的策略提取污染物,包括盐析分配和分散固相萃取以进一步净化。为了最大限度地提高通量和提取效率,最初采用Plackett-Burman设计筛选显著变量。并基于中心复合设计进行响应面法以详细实现最佳条件:乙腈中3.35%(v/v)的甲酸、1.2 g氯化钠、0.5 g无水醋酸钠、300 mg C18和140 mg伯仲胺。在优化条件下,验证中的分析特性令人满意,在准确度方面(霉菌毒素和喹诺酮类为70%-105%,磺胺类为55%-80%,其他兽药为40%-105%)、精密度(日内相对标准偏差<14%)和灵敏度(定量限范围为0.01 μg/kg至31 μg/kg)。通过使用基质匹配校准曲线评估并补偿基质效应(R>0.987)。在实际应用中,用建立的方法对45个鸡蛋和30个牛奶样品进行了检测,其中在牛奶中检测到黄曲霉毒素阳性,在鸡蛋中检测到柄曲霉素阳性。