新型纳米纤维固相萃取柱制备及其用于组织样品中柔红霉素测定研究

Preparation of Novel Packed-Nanofibers Solid Phase Extraction Column and Its Application to the Determination of Daunorubicin in Rat Tissues

研制出一种新型纳米纤维固相萃取柱,并将其用于大鼠心、肝、脾、肺、肾组织及血浆中柔红霉素的净化、浓缩处理,建立了生物样品中柔红霉素的高效液相荧光检测法。以10%(V/V)HClO4为溶剂,对组织样进行匀浆和离心处理,上清液用纳米纤维小柱净化富集,以50 mL含1%(V/V)冰醋酸的甲醇洗脱,进样20 mL检测。流动相为甲醇-水-冰醋酸(60∶40∶0.25,V/V,pH 5.5),流速为1.0 mL/min。在5种组织中,方法的定量线性范围为0.02～20 mg/g,在血浆中为0.01～1 mg/L。方法的回收率为82.7%～112.3%,日内RSD为2.0%～9.9%,日间RSD为5.2%～11.9%。本方法具有快速、灵敏等优点,可应用于动物的各组织样中柔红霉素检测。

A novel packed-nanofibers solid-phase extraction column has been investigated for purification and enrichment of daunorubicin in plasma and different tissues of rat（heart,liver,spleen,lung,kidney）.Meanwhile,an HPLC method with fluorescence detection for determination of biological samples has been deve-loped.10%（V/V） HClO4 was used to extract daunorubicin from biological samples.After homogenizing for 1min and centrifuging for 10 min at 12000 r/min,the supernatant was purified and preconcentrated by the column,then only 50 mL of eluant（methanol-acetic acid（99 ∶ 1,V/V）） was required to desorb the target compounds.The mobile phase was methanol-water-acetic acid（60 ∶ 40 ∶ 0.25,V/V,pH 5.5）,the flow rate was 1.0 mL/min.Results indicated that the linear range of daunorubicin was 0.02-20 mg/g in the tissues samples and 0.01-1.00 mg/L in the plasma samples.The recoveries were in the range of 82.7%-112.3%.RSDs for intra-day and inter-day were 2.0%-9.9% and 5.2%-11.9% respectively.The method is rapid and sensitive,which can be applied to determine daunorubicin in biological samples.