高效液相色谱法测定兔肌肉组织顺式阿曲库铵浓度

目的建立兔肌肉组织顺式阿曲库铵浓度的高效液相色谱紫外检测法。方法取单次静脉注射顺式阿曲库铵后兔膈肌和胫骨前肌,经匀浆、萃取后检测。色谱柱为Spher-sorb SCX(4.6 mm×150 mm,5μm,Phenomenex,USA),流动相为乙腈、硫酸钠和硫酸的混合液,梯度洗脱,流速:1 ml.min-1,柱温为室温;紫外检测波长为280 nm。结果顺式阿曲库铵线性范围0.1～2.0μg.g-1,最低检测限10 ng.g-1,不受肌肉组织内源性物质干扰,回收率大于90.0%,日内、日间变异率均小于5.0%,冻融稳定性良好。结论该方法特异性强,检测限低,灵敏度高,适于兔肌肉组织顺式阿曲库铵残留浓度检测。

Determination of cisatracurium in muscle tissues of rabbits by high performance liquid chromatography

Aim To establish a method by high performance liquid chromatography(HPLC) coupled with ultraviolet detection for determining cisatracurium in muscle tissues of rabbits.Methods 7 rabbits were anesthetized with pentobarbital and administered a bolus dose of cisatracurium(0.4 mg·kg-1) intravenously.Cisatracurium was extracted from tissue homogenates of diaphragm and tibialis anterior muscles using a liquid-liquid extraction followed by reverse-phase ion pairing solid-phase extraction.The eluates were then evaporated to dryness under a stream of nitrogen at 55℃.The dry samples were reconstituted with brief sonication and vortexing in heptafluorobutyric acid,and then centrifuged.The supernatants were ready for HPLC.A Sphersorb SCX column was used at room temperature,the mobile phase was composed of Na2SO4,H2SO4 and acetonitrile,using a stepwise gradient.The solvent flow rate was 1 ml·min-1 and the ultraviolet detective wavelength was 280 nm.Results The detected data were highly related to the detected concentrations.The linear range was 0.1~2.0 μg·g-1,the limit of detection was 10 ng·g-1,the relative standard deviations(RSD) of intra-day and inter-day assays were less than 5.0%.Besides,the recovery rate was more than 90.0%.Conclusion This assay proves to be simple,sensitive and precise for measuring of residual cisatracurium in muscle tissues of rabbits.