液相色谱-串联质谱法测定葡萄酒中赭曲霉毒素A、B的残留量

Determination of Residues of Ochratoxin A and B in Wine by LC-MS/MS

采用液相色谱-串联质谱法测定葡萄酒中赭曲霉毒素A、B的残留量。样品用氨水调节pH后离心,上清液过C18固相萃取柱净化,以甲醇洗脱,氮气吹至近干后用甲醇-0.15%甲酸（7＋3）溶液定容至1mL。以Agilent Eclipse XDB-C18色谱柱为分离柱,以甲醇-含5mmol·L^-1乙酸铵溶液的0.15%甲酸溶液（7＋3）混合液为流动相进行洗脱,采用电喷雾离子源及选择多反应监测模式进行测定。赭曲霉毒素A、B的线性范围在10.0μg·L^-1以内,方法的测定下限（10S/N）均为2.0μg·L^-1。对空白样品进行加标回收试验,回收率在66.3%~87.4%之间,测定值的相对标准偏差（n=6）在5.2%~7.6%之间。方法用于葡萄酒中赭曲霉毒素A、B的测定,结果与美国化学家协会检测方法的测定结果一致。

A method of LC-MS/MS was applied to determine residues of ochratoxin A and B in wine.The sample was centrifuged after pH was adjusted.The supernatant was purified using C18 SPE column with methanol as eluent.The eluate was evaporated to dryness by N2 blowing,and the residue was dissolved in 1mL of mixture of methanol-0.15%（φ）formic acid（7＋3）solution.Agilent Eclipse XDB-C18 column was used as stationary phase and the mixture of methanol-0.15%（φ）formic acid（7＋3）solution（with 5mmol·L^-1 NH4Ac）was used as mobile phase for elution.ESI and MRM were adopted in MS/MS detection.The linearity ranges of ochratoxin A and B were found below 10.0μg·L^-1,with lower limits of determination（10S/N）of 2.0μg·L^-1.Recovery measured by standard addition method was in the range of 66.3%-87.4% with RSD′s（n=6）in the range of 5.2%-7.6%.The method was applied for the determination of residual of ochratoxin A and B in wine,giving results consistent with that obtained by the AOAC method.