超高效液相色谱-串联质谱法检测猪肉中多兽药残留

Determination of Veterinary Drugs in Porcine Muscle by UPLC-MS/MS Method

摘要:

建立一种超高效液相色谱-串联质谱（ultra performance liquid chromatography/tandem mass spectrometry，UPLC-MS/MS）法同时检测猪肉中β-受体激动剂类、磺胺类、砜类抑制剂类、喹诺酮类、糖皮质激素类以及大环内酯类等20种兽药残留。待测药物使用80%体积分数的乙腈水溶液提取，经固相萃取小柱净化和氮气吹干后使用体积分数10%甲醇水进行复溶，复溶液经微孔滤膜过滤后进行UPLC-MS/MS测定。使用BEH C₁₈色谱柱梯度洗脱分离，选用电喷雾电离源，正离子扫描及多反应监测模式测定。20种药物检出限（limit of detection，LOD）在0.5～5 μg/kg之间，定量限（limit of quantitation，LOQ）在1.7～16.7 μg/kg之间，当加标水平为1、5、10 μg/kg时，平均回收率在62.1%～118.3%范围内，相对标准偏差（relative standard deviation，RSD）在0.4%～16.7%范围内。

Abstract:

An ultra performance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS) method was established for the simultaneous determination of 20 kinds of veterinary drug residues of β-receptor activitors, sulfonamides, sulfone inhibitors, quinolones, glucocorticoids and macrolides in porcine muscle. The drugs were extracted with 80% acetonitrile, purified by the solid-phase extraction cartridge, dissolved with 10% methanol after nitrogen blowing, and detected by UPLC-MS/MS after filtering by microfiltration membrane. The BEH C₁₈ column was used for the separation by gradient elution. The identification was achieved by electrospray ionization in positive mode and multiple reaction monitoring. The limit of detection(LOD) was from 0.5 to 5 μg/kg and the limit of quantitation(LOQ) was from 1.7 to 16.7 μg/kg, the recovery rate range was between 62.1%~118.3% and the relative standard deviation(RSD) was 0.4%~16.7% when the added standard substance concentration was 1, 5, 10 μg/kg.