【摘要】 建立了原乳中活性β-内酰胺酶拮抗剂的快速高分离液相色谱-串联质谱(RRLC-MS/MS)检测方法。利用活性β-内酰胺酶能够酶解青霉素族药物的特性,在原乳中加入适量氨苄青霉素,酶解1h后,检测原乳中氨苄青霉素酶解率,定性检测活性目标物。试样中氨苄青霉素经乙腈溶液提取,HLB固相萃取柱净化和浓缩后,RRLC-MS/MS多反应监测模式定性与定量分析。本方法对活性β-内酰胺酶检出限为4U/mL;对原乳中添加1mg/kg水平氨苄青霉素的加标回收率为92.3%～95.5%;相对标准偏差RSD≤10%(n=6)。本方法的定性结果与生物杯碟法完全一致。更多还原

【Abstract】 A rapid resolution liquid chromatography-tandem mass spectrometric method (RRLC-MS/MS) has been developed for the qualitative analysis of active beta-lactamases in milk samples. Penicillin was added to the samples solution to enzymolyze the active beta-lactamases. Then,the analytes were extracted by CH3CN-H2O from homogenized samples,and the extract was cleaned by Oasis HLB solid phase extraction cartridge. Quantification of penicillin was achieved by RRLC-MS/MS with multiple reaction monitoring. Detection limit of active beta-lactamases was 4 U/mL,the mean recoveries were in the range of 92.3%-95.5%,and the RSD was less than 10%(n=6). The results of this method were consistent with these by the cylinder plate method.更多还原