液相色谱-串联质谱法测定葡萄酒中赭曲霉毒素A

Determination of ochratoxin A in wine by LC-MS/MS

以赭曲霉毒素B为内标物,建立了应用固相萃取-液相色谱-串联质谱法（SPE-LC-MS/MS）对葡萄酒中赭曲霉毒素A残留量测定的方法.葡萄酒样品经过调节pH值至7.0和C18固相萃取净化的前处理过程后,采用液相色谱-串联质谱法进行测定（正离子方式,多反应监测模式）.方法定量限（LOQ）为2.0g/L.内标法定量计算,在0～10g/L质量浓度范围内线性相关系数＞0.998.在葡萄酒中分别进行2.0g/L、4.0g/L和8.0g/L三个添加水平的测试,该检测方法回收率范围97.6％～109.7％,相对标准偏差（RSD）3.0％～4.6％.方法简便、快速、准确,可用于葡萄酒中赭曲霉毒素A的定量测定.

Using ochratoxin B as internal standard substance, the application of SPE-LC-MS/MS for determination of ochratoxin A in wine sample was established. The sample was adjusted to pH 7.0 and purified with C18 solid phase extraction pretreatment process. The quantitative detection was carried out by LC-MS/MS, using a positive-ion electrospray ionization in multiple reaction monitoring mode, and the limits of quantification was 2.0 g/L. The working curves were linear in the range of 0-10 g/L, and the correlation coefficients were more than 0.998. Ochratoxin A addition in 2.0 g/L, 4.0 g/L and 8.0 g/L levels was added and the recovery rate ranged from 97.6% to 109.7% with relative standard deviations between 3.0% and 4.6%. This method was simple, rapid, accurate and adapted to confirm residues of ochratoxin A in wine.