超高效液相色谱-电喷雾电离-串联质谱法测定猪粪便中6种抗生素残留的基质效应研究

发布时间：2018-06-05 15:15

本文选题：基质效应 + 离子抑制率　；参考：《分析测试学报》2017年08期

【摘要】：基质效应普遍存在于液质联用分析中。该文通过评价"离子抑制率"指标,系统考察了应用超高效液相色谱-电喷雾电离-串联质谱法(UPLC-ESI-MS/MS)测定猪粪便中二甲氧苄啶、磺胺对甲氧嘧啶、恩诺沙星、环丙沙星、金霉素、泰乐菌素6种抗生素残留的基质效应。样品经McIlvaine-Na_2EDTA缓冲溶液提取后,采用HLB固相萃取柱净化,浓缩富集后用0.1%甲酸-甲醇溶液(85∶15,体积比)溶解。经SB C_(18)RRHD色谱柱分离,以甲醇-0.1%甲酸为流动相进行梯度洗脱,在正离子电喷雾下采用多反应监测模式检测。结果表明,猪粪便基质对6种抗生素的测定存在基质增强效应。采用基质匹配标准曲线校正法并优化样品处理条件可以对基质效应产生的影响进行补偿与消除。该研究为提高检测结果的准确度与精密度提供了借鉴。
[Abstract]:The matrix effect is widely used in liquid-mass spectrometry. The determination of dimethoprim, sulfamethoxine, enrofloxacin, ciprofloxacin, chlortetracycline in pig feces by UPLC-ESI-MS / MSM was systematically studied by evaluating the index of "ion inhibition rate" by ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS). Matrix effect of 6 antibiotic residues of tylosin. The samples were extracted by McIlvaine-Na_2EDTA buffer solution, purified by HLB solid-phase extraction column, concentrated and dissolved in 0.1% formic acid-methanol solution (85: 15, volume ratio). After separation by SB C_(18)RRHD column, gradient elution was carried out with methanol-0.1% formic acid as mobile phase, and detected by multi-reaction monitoring mode under positive ion electrospray. The results showed that porcine fecal matrix had matrix enhancement effect on the determination of 6 antibiotics. The matrix matching standard curve correction method and the optimization of sample treatment conditions can compensate and eliminate the effect of matrix effect. This study provides a reference for improving the accuracy and precision of the detection results.
【作者单位】：上海市动物疫病预防控制中心;
【基金】：上海市科技兴农重点攻关项目[沪农科攻字(2011)第4-9号]资助
【分类号】：O657.63;S859.8

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