HPLC法测定莫西沙星血药浓度  

Determination of moxifloxaxin in human plasma by HPLC

作　　者：徐玉红[1] 李玉珍[1] 唐利娟 李杰[1] 姚苑梅[1] 

机构地区：[1]广东医学院附属深圳福田人民医院药剂科,深圳518033 [2]深圳市福田区中医院手术室,深圳518034

出　　处：《中国临床药学杂志》2010年第3期149-152,共4页Chinese Journal of Clinical Pharmacy

基　　金：深圳市科技计划(医疗卫生类;编号200803147)

摘　　要：目的建立测定人血浆中莫西沙星浓度的HPLC法。方法以Kromasil C_8柱为色谱柱,含1%三乙胺的0.02 mol·L^(-1)磷酸二氢钾缓冲液(用磷酸调节pH至3.0):甲醇:乙腈(65:20:15,V/V/V)为流动相,流速1 mL·min^(-1),柱温30℃,检测波长296nm,进样量20μL,内标为加替沙星。血样以二氯甲烷提取,氮气流吹干后以流动相复溶进样。结果加替沙星、莫西沙星保留时间分别约为5.8、7.6 min,莫西沙星在血药浓度0.05～5.0 mg·L^(-1)内线性关系良好(r=0.999 8),最低定量限为0.05 mg·L^(-1),检测限0.015 mg·L^(-1)。方法回收率为99.37%～104.50%,提取回收率为80.48%～91.25%。日内精密度(RSD)为4.03%～5.73%,日间精密度(RSD)为4.53%～6.83%。样品在低温冷冻(-20℃)条件下至少3个月稳定。结论建立的HPLC法准确可靠,简便快速,灵敏度较高,可用于莫西沙星血药浓度测定及药动学研究。AIM To develop and validate a HPLC method for the determination of moxifloxacin concentration in human plasma. METHODS The separation was performed on a Kromasil Cs column. The mobile phase consisted of 65 % 0.02 mol. L- 1 KH2PO4 buffer solution （containing 1% triethylamine, adjusted pH to 3.0 with phosphoric acid）, 20% methanol and 15% acetonitrile （65：20： 15, V/V/V）. The flow rate was 1.0 mL.min-1 and the detection wavelength was 296 nm. The colunm temperature was 30℃ and injection volume was 20 uL. Gatifloxacin was chosen as the internal standard. The plasma was extracted with 5 mL of methylene chloride and dried under nitrogen. The residue was redissolved with mobile phase and injected into the sampler. RESULTS The retention time of gatifloxacin and moxifloxacin was about 5.8 min and 7.6 min, respectively. The calibration curve for moxifloxacin was linear in the concentration range of 0.05 - 5.0 mg.L-1. The limit of quantitation （LOQ） for moxifloxacin was 0.05 mg.L-1,and the limit of detection （LOD） was 0.015 mg. L- 1, respectively. The methodological recovery of low, medium and high concentration was 99.37% - 104.50%. The recovery of extraction was 80.48% - 91.25%. The relative standard deviations for intraday and inter-day assay were 4.03% - 5.73% and 4.53% - 6.83%, respectively. The sample was stable at least within three months under - 20℃. CONCLUSION The established HPLC method is accurate and sensitive. It could be used for the determination of moxiflocacin concentration in human plasma and its phannacokinetic study.

关 键 词：莫西沙星 高效液相色谱 血药浓度 

分 类 号：R96[医药卫生—药理学]