摘要
目的:建立高效液相色谱法测定血清和尿中加替沙星药物浓度。方法:采用 ODS-C_(18)柱(150 mm×4.6 mm,5μm,迪马公司),以0.008 mol·L^(-1)磷酸(2 mol·L^(-1)氢氧化钠溶液调 pH 为3.0)-乙腈(80:20,v/v,含0.005 mol·L^(-1)四丁基溴化铵)为流动相;血清及尿样品经10%三氯乙酸沉淀去蛋白后上柱分析。用内标法对加替沙星进行定量测定,内标物为诺氟沙星。结果:该法内标物和加替沙星出峰时间分别为2.8 min 和4.4 min,分离系数 R>2,分离效果好;加替沙星质控3种浓度(0.06,0.36,1.2 mg·L^(-1))日内、日间的 RSD,血清样品小于10%,尿样品小于7.6%;血清回收率为94.7%～105.6%,尿回收率为94.7%～98.8%;血清样品线性范围为0.015～2.4 mg·L^(-1),相关系数为0.9995,尿样品线性范围为0.015～4.8 mg·L^(-1),相关系数为0.9999;血清、尿样品加替沙星最低检出限分别为0.015及0.007 mg·L^(-1)。结论:HPLC 测定血清及尿中加替沙星浓度,准确、特异、稳定、灵敏,可用于相关研究。
Objective： To establish an HPLC method to detect the concentration of gatifloxacin in human serum and urine. Methods： ODS- C18 culumn（ 150 mm ×4. 6 mm,5 μm）and a mixture of 0. 008 mol · L^-1 phosphoric acid （ adjusted pH to 3.0 with 2 mol · L^-1 sodium hydroxide solution ） and acetonitrile （ 80 ： 20, v/v） containing 0. 005 mol · L^-1 tetrabutylammonium bromide were used as the fix and mobile phases respectively. Norfloxacin was used as the internal standard. The serum and urine samples were pretreated with 10% trichloroacetic acid for removing of protein. Results： In the HPLC conditions, the retention times for gatifloxacin and norfloxacin were 4. 4 min and 2. 8 min respectively. With three quality control concentrations of 0. 06,0. 36,1.2 mg L^-1, the accuracy and precision of the assay were satisfactory. Both the within - day and between - day RSD were less than 10% or 7. 6% for serum or urine. The recovery rates were 94. 7% - 105.6% for serum and 94. 7% - 98.8% for urine. The standard calibration curves of concentrations and peak area were linear in the concentration ranges of 0. 015 - 2. 4 mg L^-1 and 0. 015 -4. 8 mg L^-1 and the correlation coefliciencies were 0. 9995 and 0. 9999 for serum and urine respectively. The minimum detective limits were 0. 015 mg L^-1 in serum and 0. 007 mg L^-1 in urine. Condnsion： This HPLC method is accurate, stable and sensitive in the measurment of the concentrations of gatifloxacin in serum and urine and can be applied in clinical pharmacology study.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2006年第7期990-992,共3页
Chinese Journal of Pharmaceutical Analysis
