Carretero I, Vadillo J M, Laserna J J
Department of Analytical Chemistry, Faculty of Sciences, University of Málaga, Spain.
Analyst. 1995 Jun;120(6):1729-32. doi: 10.1039/an9952001729.
A rapid solid-phase extraction (SPE) procedure was developed for the quantitative isolation of three important antipyrine (dipyrone) metabolites from human plasma: 4-formylaminoantipyrine (FAA), 4-aminoantipyrine (AA) and 4-methylaminoantipyrine (MAA). Separation and quantitation were performed using micellar liquid chromatography (MLC) with a 0.1 mol l-1 sodium dodecyl sulfate (SDS)-2.5% pentanol mobile phase and UV detection at 262 nm. The metabolites were well resolved in less than 5 min using an octadecyl silica-bonded stationary phase. The extraction procedure involved passing 0.3 ml of plasma sample through a disposable SPE cartridge packed with C18 bonded porous silica. The adsorbed metabolites were removed from the cartridge with methanol. The eluent was evaporated to dryness and the residue was reconstituted with mobile phase and injected into the chromatographic system. The cartridge blank interferent peaks, the effects on reproducibility of sample loading in the cartridge and volume needed for desorption of metabolites were evaluated. The concentration of metabolites ranged between 2.4 and 4 micrograms ml-1. The present procedure yields recoveries for the three metabolites ranging from 93 to 100%. The relative standard deviation (Sr) ranged between 1.2 and 13.6%. Limits of detection (LODs) were 10.5, 11.5 and 17.0 ng ml-1 for FAA, AA and MAA, respectively.
开发了一种快速固相萃取（SPE）方法，用于从人血浆中定量分离三种重要的安替比林（安乃近）代谢物：4-甲酰氨基安替比林（FAA）、4-氨基安替比林（AA）和4-甲基氨基安替比林（MAA）。使用胶束液相色谱（MLC），以0.1 mol l-1十二烷基硫酸钠（SDS）-2.5%戊醇为流动相，并在262 nm处进行紫外检测，进行分离和定量。使用十八烷基硅胶键合固定相，在不到5分钟的时间内，代谢物得到了很好的分离。萃取过程包括将0.3 ml血浆样品通过装有C18键合多孔硅胶的一次性SPE小柱。用甲醇从柱上洗脱吸附的代谢物。将洗脱液蒸发至干，残渣用流动相复溶后注入色谱系统。评估了柱空白干扰峰、柱中进样量对重现性的影响以及代谢物解吸所需的体积。代谢物浓度范围在2.4至4微克/毫升之间。本方法对三种代谢物的回收率在93%至100%之间。相对标准偏差（Sr）在1.2%至13.6%之间。FAA、AA和MAA的检测限（LOD）分别为10.5、11.5和17.0纳克/毫升。
