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采用高效液相固相萃取提取和分析大肠癌细胞SW480-B7和SW480-NC及血浆中5-Fu的含量,提高了萃取效率。优化色谱条件,在流动相中添加三氟乙酸改善了峰型,提高了理论塔板数。色谱柱:Diamonsil C18柱(5μm,4.6×250 mm),流动相:0.08%磷酸水溶液(含0.15%三氟乙酸)-甲醇溶液(体积比95:5),检测波长266 nm。血浆样本线性范围0.025~25μg/m L,检出限0.02μg/m L(S/N≥3),回归方程为Y=34783X+34562(R~2=0.9991);癌细胞线性范围0.03125~12.5μg/m L,最小检测浓度0.025μg/m L(S/N≥3),回归方程为Y=37963X+36842(R2=0.9993)(SW480-B7);Y=30244X+32421(R2=0.9998)(SW480-NC);所有样品回收率在86%~102%之间,日内RSD和日间RSD分别小于5%和8%。
The extraction and analysis of 5-Fu in SW480-B7 and SW480-NC and plasma by high performance liquid phase solid-phase extraction (SPE-HPLC) were carried out to improve the extraction efficiency. Optimization of chromatographic conditions, the addition of trifluoroacetic acid in the mobile phase improved the peak shape and increased the theoretical plate number. The chromatographic column was Diamonsil C18 column (5μm, 4.6 × 250 mm). The mobile phase consisted of 0.08% phosphoric acid solution (containing 0.15% trifluoroacetic acid) -methanol solution (volume ratio 95: 5) The linear range of plasma samples was 0.025 ~ 25μg / mL with a detection limit of 0.02μg / mL (S / N≥3). The regression equation was Y = 34783X + 34562 (R ~ 2 = 0.9991) The regression equation was Y = 37963X + 36842 (R2 = 0.9993) (SW480-B7); Y = 30244X + 32421 (R2 = 0.9998) and the minimum detection concentration was 0.025μg / (SW480-NC). The recoveries of all samples ranged from 86% to 102%. The intraday RSD and daytime RSD were less than 5% and 8%, respectively.