液相色谱-串联质谱法检测水产品中磺胺类和喹诺酮类药物残留

Determination of Residual Sulfas and Quinolones in Aquatic Products by HPLC-MS/MS Using Deuterium Reagent as Internal Standard

建立了高效液相色谱-串联质谱（HPLC-MS／MS）法检测水产品中磺胺类、喹诺酮类等合成抗菌剂残留的方法：样品以乙腈为提取剂，提取物经脱脂、净化、浓缩后，用流动相溶解。用氘代试剂内标法定量，高效液相色谱-串联质谱法测定。本方法通过梯度洗脱将12种磺胺类、喹诺酮类进行良好分离。标准曲线线性范围0．05～0．8mg／L，线性相关系数r=0．9875～0．9991，回收率为61％～104％，相对标准偏差（RSD）为4．75％～6．12％（n=5），检出限为10～50μg/kg。

This paper describes an HPLC - MS/MS method for the determination of residual sulfas and quinolones in aquatic products. The antibiotics in the samples were extracted with acetonitrile, and the extracts were defatted and purified using hexane and then concentrated by evaporation. The residues were dissolved in the mobile phase. Sulfas and quinolones were well separated using gradient elution. The antibiotics were detected by HPLC - MS/MS and the deuterium reagent was used as internal stand- ard. The linearity of standard curves was maintained in the range of 0.05 - 0. 8 mg/L, with the regression coefficients r = 0. 987 5 - 0. 999 1. The average recoveries from laboratory spiking experiments were 61%- 104% , with relative standard deviations of 4.75%- 6. 12% （n = 5 ）. The quantitation limits were 10-50 μg/kg.