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目的建立测定人血清中环丙沙星浓度的高效液相色谱方法。方法血清样品经5%高氯酸沉淀蛋白。色谱柱为Eclipse XDB-C18柱(150 mm×4.6mm,5μm),流动相为乙腈-0.025 mol·L~(-1)磷酸溶液(用三乙胺调p H至3.0)=15∶85,流速为1.0 m L·min~(-1);柱温为40℃,检测波长为278 nm,加替沙星为内标。结果环丙沙星在0.05~50.00μg·m L~(-1)线性关系良好(r>0.999 5);低、中、高质量浓度质控样品(0.1,1.0,4.0μg·m L~(-1))的日内相对标准偏差(RSD)为0.98%~2.63%,日间RSD为1.87%~3.16%,绝对回收率为49.2%~54.7%。结论本法有良好的特异性、灵敏度、精密度和准确度,适用于临床患者的血药浓度测定。
Objective To establish a high performance liquid chromatographic method for the determination of ciprofloxacin in human serum. Methods Serum samples were precipitated with 5% perchloric acid. The column was an Eclipse XDB-C18 column (150 mm × 4.6 mm, 5 μm) with a mobile phase of acetonitrile-0.025 mol·L -1 phosphoric acid (p H = 3.0 with triethylamine) = 15:85, The flow rate was 1.0 m L · min -1. The column temperature was 40 ℃, the detection wavelength was 278 nm, and gatifloxacin was the internal standard. Results Ciprofloxacin had a good linearity (r> 0.999 5) at 0.05 ~ 50.00 μg · m L -1; low, medium and high quality control samples (0.1, 1.0, 4.0 μg · m L ~ -1)) was 0.98% -2.63%, daytime RSD was 1.87% -3.16%, and the absolute recovery was 49.2% -54.7%. Conclusion This method has good specificity, sensitivity, precision and accuracy, suitable for the determination of blood concentration in clinical patients.