CAJ | 학술논문

建立了一种猪肝中26种β2-受体激动剂药物残留的反相液相色谱-串联质谱( HPLC-MS/MS)检测方法。样品经β-葡萄糖苷酸酶/芳基硫酸酯酶酶解12 h 后,加入 HClO4调至 pH 1,去除蛋白,残渣经过0.1 mol/L HClO4再次提取后,合并提取液,调节混合提取液至pH 4,过混合阳离子( MCX)固相萃取柱净化。采用0.1%甲酸(A)和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱,质谱(ESI+)采用多离子检测模式( MRM)对β2-受体激动剂的定量离子和定性离子进行监测,本方法在15 min内完成26种目标化合物的分离分析。26种β2-受体激动剂在5、10和20μg/L添加水平的回收率为64.0%~112.7%,相对标准偏差小于15.2%,方法检出限为0.15~1.35μg/kg。
건립료일충저간중26충β2-수체격동제약물잔류적반상액상색보-천련질보( HPLC-MS/MS)검측방법。양품경β-포도당감산매/방기류산지매매해12 h 후,가입 HClO4조지 pH 1,거제단백,잔사경과0.1 mol/L HClO4재차제취후,합병제취액,조절혼합제취액지pH 4,과혼합양리자( MCX)고상췌취주정화。채용0.1%갑산(A)화0.1%갑산-을정(B)작위류동상진행제도세탈,질보(ESI+)채용다리자검측모식( MRM)대β2-수체격동제적정량리자화정성리자진행감측,본방법재15 min내완성26충목표화합물적분리분석。26충β2-수체격동제재5、10화20μg/L첨가수평적회수솔위64.0%~112.7%,상대표준편차소우15.2%,방법검출한위0.15~1.35μg/kg。
A method for determination of residues of 26 β2-agonists in pork liver was developed using high performance liquid chromatography with tandem mass spectrometric ( HPLC-MS/MS ) . After enzymatic hydrolysis with β-Glucuronidase/Arylsulfatase for 12 hours, the pH of sample solution was adjusted to 1 using perchloric acid for protein precipitation. The precipitate was extracted with 0. 1mol/L perchloric acid aqueous. The extracts in the above two steps were combined and adjusted to pH 4 for the solid phase extraction ( MCX) . And then the 26 β2-agonists residues in the extracts were separated on a reversed phase HPLC column using a gradient elution program of 0. 1% formic acid aqueous solution (A) and 0. 1% formic acid in acetonitrile solution ( B) . Multiple reaction monitoring ( MRM) with positive polarity was selected to monitor qualitative and quantitative ion. Based on the optimized method, 26 β2-agonists could be analyzed in 15 min. The recoveries ranged from 64 . 0% to 112 . 7% for the 26 kinds ofβ2-agonists residues with three spiked levels of 5, 10 and 20 μg/kg. The relative standard deviations ( RSDs) were less than 15. 2%. The limits of detection (LOD) for the 26 kinds of β2-agonists were 0. 15-1. 35 μg/kg.