Luo Huitai, Xie Mengting, Huang Xiaolan, Wu Huiqin, Zhu Zhixin, Huang Fang, Lin Xiaoshan, Ouyang Gangfeng
Se Pu. 2015 Apr;33(4):354-62. doi: 10.3724/sp.j.1123.2014.12005.
A novel multiresidue analytical method has been developed and validated for the determination of five classes of veterinary drugs including 18 β-lactams, 15 quinolones, 21 sulfonamides, 3 sulfonamide potentiators and 6 antiparasitics in meat using dispersive solid-phase extraction (dispersive-SPE) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The analytes were extracted with a vortex mixer by 0.1 mol/L Na2 EDTA solution and acetonitrile containing 1% (v/v) acetic acid, and then the extracts were purified using dispersive-SPE with C18 sorbent. Electrospray ionization mass spectrometry was operated in positive mode using dynamic multiple reaction monitoring (DMRM) for the qualitative and quantitative analysis of the 63 analytes after the separation on a Poroshell EC-C18 column (100 mm x 2.1 mm, 2.4 µm). The correlation coefficients of linear calibration curves were over 0.99 in the corresponding concentration ranges. The average recoveries of the 63 analytes ranged from 62.2% to 112.0%, and the relative standard deviations (RSDs) were 3.1%-16.3% in spiked meat (pork, beef and chicken muscle) at three levels. The limits of detection (LODs, S/N ≥ 3) and the limits of quantification (LOQs, S/N ≥ 10) were 0.1-3.0 µg/kg and 0.5-10.0 µg/kg, respectively. The method is simple, rapid, sensitive, reliable and suitable for the determination of residues in animal products.
已开发并验证了一种新型多残留分析方法,用于测定肉类中的五类兽药,包括18种β-内酰胺类、15种喹诺酮类、21种磺胺类、3种磺胺增效剂和6种抗寄生虫药,该方法采用分散固相萃取(dispersive-SPE)和高效液相色谱-串联质谱(HPLC-MS/MS)。用0.1 mol/L Na2 EDTA溶液和含1%(v/v)乙酸的乙腈通过涡旋混合器提取分析物,然后用C18吸附剂的分散固相萃取法对提取物进行净化。在Poroshell EC-C18柱(100 mm×2.1 mm,2.4 µm)上分离后,采用动态多反应监测(DMRM)以正模式运行电喷雾电离质谱,对63种分析物进行定性和定量分析。线性校准曲线在相应浓度范围内的相关系数均超过0.99。在加标肉(猪肉、牛肉和鸡肉肌肉)的三个浓度水平下,63种分析物的平均回收率为62.2%至112.0%,相对标准偏差(RSD)为3.1%-16.3%。检测限(LOD,S/N≥3)和定量限(LOQ,S/N≥10)分别为0.1-3.0 µg/kg和0.5-10.0 µg/kg。该方法简便、快速、灵敏、可靠,适用于动物产品中残留物的测定。