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目的建立反相高效液相色谱法(RP-HPLC)测定人血浆及尿中头孢唑兰浓度。方法采用Welch Materials XB C18(4.6mm×150 mm,5μm)色谱柱,血样及尿样流动相分别为乙腈-0.01 mol.L-1醋酸钠-三乙胺(6∶94∶0.001,醋酸调pH为3.52)和乙腈-0.01 mol.L-1醋酸钠-三乙胺(3∶97∶0.001,醋酸调pH为3.55),检测波长为235 nm。血浆样品加乙腈沉淀蛋白后再用二氯甲烷反复洗后进样,内标为氟苷。尿样用纯水直接稀释后进样,外标法定量。结果血浆样品标准曲线在0.15~307.2 mg.L-1范围内线性关系良好,最低定量浓度为0.15 mg.L-1,预处理回收率为86.9%~108.4%,批内及批间RSD分别小于2.4%和5.4%。尿样标准曲线在4.69~4 800 mg.L-1内线性关系良好,最低定量浓度为4.69 mg.L-1,批内及批间RSD分别小于3.0%和5.9%。结论本法具有快速简便,灵敏准确等特点,适用于血浆及尿中头孢唑兰浓度测定。
Objective To establish a reverse-phase high-performance liquid chromatography (RP-HPLC) determination of cefazolin concentration in human plasma and urine. Methods The mobile phase of blood sample and urine sample were acetonitrile-0.01 mol·L-1 sodium acetate-triethylamine (6:94:0.001, pH adjusted by acetic acid) using Welch Materials XB C18 column (4.6 mm × 150 mm, 3.52) and acetonitrile-0.01 mol. L-1 sodium acetate-triethylamine (3:97:0.001, pH 3.55). The detection wavelength was 235 nm. Plasma samples were precipitated with acetonitrile and then repeatedly washed with dichloromethane after injection, the internal standard for the fluorine glycosides. Urinary samples directly diluted with pure water after injection, external standard method. Results The calibration curves of plasma samples showed a good linearity in the range of 0.15-370.2 mg.L-1 with the lowest concentration of 0.15 mg.L-1 and the recovery of pretreatment was 86.9% -108.4%. The intra-assay and inter-assay RSD were less than 2.4% and 5.4%. The standard curve of urine samples showed a good linearity in the range of 4.69-4 800 mg · L-1 with the lowest concentration of 4.69 mg · L-1. The intra-and inter-assay RSD were less than 3.0% and 5.9%, respectively. Conclusion This method is rapid, simple, sensitive and accurate. It is suitable for the determination of cefazolin in plasma and urine.