新型二维液相色谱测定百草枯尿液浓度的研究

发布时间：2018-02-24 16:06

  本文关键词： 百草枯 二维液相色谱法 尿液 自动化　出处：《中国药学杂志》2017年10期 　论文类型：期刊论文

【摘要】：目的采用新型二维液相色谱系统(2D-LC-UV)建立中毒患者尿液中百草枯浓度的测定方法,并对二维色谱特征及方法学进行评估。方法 2D-LC-UV由第一维和第二维液相色谱系统及FLC转运机构构成,尿液100μL直接进样,在第一维Aston SX1色谱柱(4.6 mm×250 mm,5μm)上进行在线富集及初级分离,通过Aston SX捕集柱(4.6 mm×100 mm,5μm)捕集保留,最后转移到第二维色谱柱Aston SX1(4.6 mm×75 mm,5μm)上进一步分离检测。第一维流动相为2 mol·L~(-1)醋酸铵-乙腈=10∶1(V∶V),流速1.0 mL·min~(-1),捕集柱流动相为纯水,第二维流动相为2.5 mol·L~(-1)醋酸铵-甲醇-乙腈=5∶3∶1(V∶V∶V),流速1.0 mL·min~(-1),柱温40℃,紫外检测波长285 nm。结果所建立的二维色谱方法可以去除样品中大部分杂质,最大可以在线处理500μL样品,目标物在二维系统中转移完整;在20~20 000ng·mL~(-1)内线性关系良好(r=0.999 9),不同来源尿液中未发现干扰;工作曲线可长时间稳定,色谱平衡时间小于15min。结论本方法稳定性良好、简便快速、结果准确、自动化程度高,不依赖于专门的技术人员,适用于临床百草枯中毒患者的快速检测,为临床制定解救方案提供科学依据。
[Abstract]:Objective to establish a new two-dimensional liquid chromatographic system, 2D-LC-UV, for the determination of paraquat concentration in urine of poisoning patients. Methods 2D-LC-UV was composed of first and second dimensional liquid chromatography system and FLC transporter. Urine was directly injected with 100 渭 L urine. The sample was preenriched on the first dimensional Aston SX1 column (4.6 mm 脳 250mm / 5 渭 m), and the primary separation was performed on the first dimensional Aston SX1 chromatographic column (4.6mm 脳 250mm / 5 渭 m). Aston SX trapping column (4.6mm 脳 100mm-1 渭 m) was used for further separation and detection. The mobile phase was 2 mol 路L ~ (-1) acetonitrile (10: 1) with a flow rate of 1.0 mL 路min ~ (-1) 路min ~ (-1). The mobile phase of the column was pure water, and the flow rate was 1.0 mL 路min ~ (-1) 路min ~ (-1). The second mobile phase is 2.5 mol 路L ~ (-1)) ammonium acetate, methanol-acetonitrile, 5: 3: 1: 1: v: v: v, flow rate 1.0 mL 路min ~ (-1), column temperature 40 鈩，

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