在线固相萃取-高效液相色谱法同时测定人尿液中的马钱子碱和士的宁

发布时间：2018-05-25 08:24

本文选题：马钱子碱 + 士的宁　；参考：《分析试验室》2017年08期

【摘要】：建立了全自动、快速的在线固相萃取-液相色谱技术用于测定人尿液中的马钱子碱和士的宁的方法。样品离心后直接进样,其中被测组分富集于Hyper Sep Retain MCX柱上,尿液中的大分子基质物质不被保留而排出,在线完成萃取和净化富集过程;再通过阀切换使待测物转移至分析流路,在Acclaim C_(18)色谱柱上分离检测。分析时间约13 min。在线固相萃取流路以0.1%H_3PO_4和乙腈为流动相,1 m L/min流速萃取和洗脱;分析流路以乙腈和0.02 mol/L KH_2PO_4为流动相,1 m L/min流速等度洗脱,检测波长为260 nm。马钱子碱在1.25×10~(-6)~2.5×10~(-4)mol/L浓度范围内相关系数r为0.9930,高、中、低浓度的平均回收率分别为85.7%,81.4%和80.9%;士的宁在2.9×10~(-6)~2.9×10~(-4)mol/L浓度范围内相关系数r为0.9993,高、中、低浓度的平均回收率分别为87.1%,82.4%和78.9%。本法可用于测定人尿液中的马钱子碱和士的宁含量。
[Abstract]:A rapid and automatic method for the determination of brucine and strychnine in human urine by on-line solid phase extraction (SPE) and liquid chromatography (LC) has been established. After centrifugation, the samples were directly injected, in which the measured components were enriched on the Hyper Sep Retain MCX column, and the macromolecular matrix substances in the urine were discharged without reservation. The process of extraction and purification and enrichment was completed online; then, the tested substances were transferred to the analytical flow path through valve switching. The method was separated and detected on Acclaim C _ S _ (18) chromatographic column. The analysis time is about 13 mins. 0.1%H_3PO_4 and acetonitrile were used as mobile phase and 1 m L/min as flow rate extraction and elution, and acetonitrile and 0.02 mol/L KH_2PO_4 as mobile phase were used as mobile phase and 1 m L/min as flow rate in on-line solid-phase extraction. The detection wavelength was 260 nm. The average recoveries of brucine were 85.71.4% and 80.9% in the range of 1.25 脳 10 ~ (-1) ~ (-6) 脳 10~(-4)mol/L ~ (2. 5) 脳 10~(-4)mol/L, respectively, and the average recoveries of strychnine in the range of 2.9 脳 10 ~ (-1) -6 ~ (2. 9) 脳 10~(-4)mol/L were 0.9993, respectively. The average recoveries of medium and low concentrations were 87.4% and 78.994%, respectively. This method can be used for the determination of brucine and strychnine in human urine.
【作者单位】：河北中医学院基础医学院;河北医科大学公共卫生学院;河北省疾病预防控制中心;
【基金】：河北省高等学校科学技术研究项目(Z2014030) 河北省食品药品监督管理局科技项目(PT2014054)资助
【分类号】：O657.72;R446.12

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