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目的:建立一种兔皮肤中全缘千里光碱测定的HPLC方法。方法:采用X-Terra RP18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-水(23∶77,以冰醋酸、氨水调节pH至7.1),流速0.8 m L·min~(-1),柱温为室温,检测波长213 nm,进样量20μL。样品处理过程包括皮肤匀浆、液-液萃取、氮气吹干有机层、残留物复溶及进样分析。结果:皮肤中的内源性物质对测定无干扰;样品皮肤(1 cm2)中药物含量在0.525~31.5μg范围内与其峰面积的线性关系良好(r=0.999 8,n=7);日内、日间精密度良好(RSD≤12.2%);准确度(相对回收率)为96.2%~105.0%,提取回收率为79.4%~83.7%;复溶的供试品溶液在24 h内稳定(相对回收率为95.2%~100.3%),皮肤样品冷冻-解冻循环3次测定结果稳定(相对回收率为96.2%~101.8%);皮肤中全缘千里光碱含量测定结果表明,应用12 h以后全皮及角质层下皮肤中药物滞留量的大小关系为:全缘千里光碱脂质体混悬液>全缘千里光碱脂质体凝胶剂>全缘千里光碱普通凝胶剂。结论:该方法的精密度、准确度、稳定性均符合生物样本测定要求,可用于兔皮肤中全缘千里光碱的测定。
OBJECTIVE: To establish a HPLC method for the determination of Trichlorethylene in rabbit skin. METHODS: The mobile phase consisted of acetonitrile-water (23:77, adjusted to pH 7.1 with glacial acetic acid and aqueous ammonia) using a X-Terra RP18 column (250 mm × 4.6 mm, 5 μm) 1). The column temperature was room temperature and the detection wavelength was 213 nm. The injection volume was 20 μL. Sample processing included homogenization of the skin, liquid-liquid extraction, drying of the organic layer with nitrogen, reconstitution of residues, and injection analysis. Results: The endogenous substances in the skin had no interference with the assay. The linearity of the sample in the skin (1 cm2) ranged from 0.525 to 31.5 μg with a good linear relationship (r = 0.999 8, n = 7) The precision was good (RSD≤12.2%) during the day; the accuracy (relative recovery) was 96.2% ~ 105.0% and the recovery rate was 79.4% ~ 83.7%; the solution of the reconstituted sample was stable within 24 h The recoveries ranged from 95.2% to 100.3%). The skin samples were frozen-thawed three times and the results were stable (relative recovery was 96.2% ~ 101.8%). The results of the determination of Trichlorethylene in the skin showed that after 12 h The skin and the stratum corneum in the skin retention of drugs in the size of the relationship as follows: Trichlorethylene Liposome Suspension> Trichlorethylene Liposome Gel Agent> Trichlorethylene alkaline gel. Conclusion: The precision, accuracy and stability of the method are in line with the requirements of biological samples, and can be used for the determination of Trichlorethylene in rabbit skin.