[Rapid determination of trace ciprofloxacin residue in milk samples using molecularly imprinted membrane extraction-high performance liquid chromatography-tandem mass spectrometry].
[Rapid determination of trace ciprofloxacin residue in milk samples using molecularly imprinted membrane extraction-high performance liquid chromatography-tandem mass spectrometry].
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DOI：
10.3724/sp.j.1123.2020.02017
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发表时间：
2020-07
期刊：
影响因子：
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通讯作者：
Hongjing Tian;Tong Liu;Song You;Feng Zhang
中科院分区：
文献类型：
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作者：
Hongjing Tian;Tong Liu;Song You;Feng Zhang
以聚偏二氟乙烯膜为载体，以恩诺沙星为模板分子，α-甲基丙烯酸为功能单体，乙二醇二甲基丙烯酸酯为交联剂，氯仿-甲醇混合溶剂为致孔剂，制备了恩诺沙星分子印迹膜。MIM对环丙沙星具有良好的选择性、较高的吸附容量和较高的吸附速率。此外，建立了分子印迹膜萃取(MIME)与高效液相色谱-串联质谱仪(LC-MS/MS)相结合的方法，用于牛奶样品中环丙沙星残留的选择性分析。样品前处理只需一步蛋白质沉淀。环丙沙星在0.1~2 0 0μg/L质量浓度范围内线性关系良好，相关系数高(R2>；0.9996)。方法检出限(S/N=3)为0.02μg/L，定量限(S/N=10)为0.1μg/L。日内精密度和日间精密度的相对标准偏差(RSD)为3.3%~7.9%。环丙沙星的回收率在92.6%~119.1%之间。结果表明，该方法简便、快速、准确度高、灵敏度高，适用于牛奶中痕量环丙沙星残留的快速检测。
An enrofloxacin (ENR) molecularly imprinted membrane (MIM) was prepared with a polyvinylidenedifluoride (PVDF) membrane as the carrier, ENR as the dummy template molecule, α-methacrylic acid (MAA) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, and a chloroform-methanol mixture solvent as the porogen. The MIM showed excellent selectivity, high adsorption capacity, and high adsorption rate for ciprofloxacin. Additionally, a method combining molecularly imprinted membrane extraction (MIME) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed and validated for the selective analysis of trace ciprofloxacin residue in milk samples. The sample pretreatment involved only a single step of protein precipitation. Ciprofloxacin showed good linearity in mass concentration range of 0.1-200 μg/L with a high correlation coefficient (r2>0.9996). The limit of detection (LOD, S/N=3) and limit of quantification (LOQ, S/N=10) were 0.02 μg/L and 0.1 μg/L, respectively. The relative standard deviations (RSDs) of interday and intraday precisions ranged from 3.3% to 7.9%. The ciprofloxacin recovery was in the range of 92.6%-119.1%. The results showed that the proposed method is simple and fast, with high accuracy and sensitivity, thus being suitable for the rapid detection of trace ciprofloxacin residue in milk samples.