分散固相萃取-超高效液相色谱-串联质谱法测定豆芽中6种喹诺酮类药物

本文建立了豆芽中恩诺沙星、环丙沙星、氧氟沙星、诺氟沙星、洛美沙星、培氟沙星6种喹诺酮类药物残留的分散固相萃取-超高效液相色谱-串联质谱的快速测定方法。豆芽样品中6种喹诺酮药物采用1%甲酸乙腈提取,提取液经N-丙基乙二胺(PSA)、十八烷基键合硅胶(C₁₈)、无水硫酸镁(MgSO₄)、石墨化碳(GCB)4种填料净化,净化液过滤膜后经ACQUITY UPLC BEH C₁₈色谱柱,甲醇-0.1%甲酸水流动相梯度分离,采用UPLC-MS/MS多反应监测模式进行测定,同位素内标法定量。结果显示:6种喹诺酮类药物在1.0~100.0 μg/L浓度范围内线性关系良好(r≥0.9982),检出限为0.1~0.3 μg/kg,定量限为0.3~1.0 μg/kg,在2、4、20 μg/kg三个浓度添加水平的回收率为96.53%~106.94%,相对标准偏差为2.73%~7.60%。该方法快速简便、灵敏度高、准确度高、重现性好,适用于豆芽样品中6种喹诺酮类药物的同时检测。

Determination of 6 Kinds of Fluoroquinolones in Bean Sprouts Based on Dispersed Solid Phase Extraction UPLC-MS/MS Method

This paper demonstrated a fast approach to test 6 kinds of fluoroquinolones(enrofloxacin,ciprofloxacin,ofloxacin,norfloxacin,lomefloxacin,pefloxacin)in bean sprouts by UPLC-MS/MS method. The sample was firstly extracted by 1% formic acid acetonitrile,the extraction solution was purified by dispersed solid phase extraction using MgSO₄,PSA,C₁₈,GCB. A gradient separation was performed on the supernatant via ACQUITY UPLC BEH C₁₈ column(mobile phase:methanol and 0.1% formic acid). The separated subjects were tested by UPLC-MS using MS Multi-Reaction-Monitor(MRM)technique,and quantified using internal standard method. The results indicated that the correlation between concentration of fluoroquinolone and signal was linear when the concentration was in the range of 1.0~100.0 μg/L. The correlation coefficient was larger than 0.9982.The limits of detection were within 0.1~0.3 μg/kg,and the limits of quantitation were within 0.3~1.0 μg/kg. The results indicated the rates were between 96.53%~106.94% when the subject concentration was 2,4 and 20 μg/kg,separately. The relative standard deviations were in the range of 2.73%~7.60%. The method is easy,fast,sensitive,accurate and stable. It is suitable for simultaneous detection of 6 kinds of fluoroquinolones in bean sprouts.