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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。
A fully automated and rapid on-line SPE-LC method was developed for the determination of brucine and strychnine in human urine. The sample is directly injected after centrifugation, wherein the tested components are enriched on a Hyper Sep Retain MCX column, the macromolecular matrix substance in the urine is discharged without being retained, and the extraction and purification and enrichment processes are completed online; The analyte is transferred to the analytical channel for detection on an Acclaim C_ (18) column. Analysis time is about 13 min. The on-line SPE column was eluted with 0.1% H 3 PO 4 and acetonitrile at a flow rate of 1 mL / min. The mobile phase consisted of acetonitrile and 0.02 mol / L KH 2 PO 4 as the mobile phase at a flow rate of 1 mL / min Elution, detection wavelength of 260 nm. The correlation coefficient r of brucine in the concentration range of 1.25 × 10 -6 ~ 2.5 × 10 -4 mol / L was 0.9930, and the average recoveries of high, medium and low concentrations were respectively 85.7% and 81.4 % And 80.9%, respectively. The correlation coefficient r of strychnine in the concentration range of 2.9 × 10 -6 ~ 2.9 × 10 -4 mol / L was 0.9993. The average recoveries of high, medium and low concentrations were 87.1%, 82.4% and 78.9%. This method can be used to determine the content of brucine and strychnine in human urine.