摘要
建立了一种同时分离7种氟喹诺酮类药物(FQs)的微乳液电动毛细管色谱(MEEKC)。用十二烷基硫酸钠(SDS)作为表面活性剂,系统考察了缓冲溶液浓度和pH、SDS、助表面活性剂和油相的浓度、温度等对分离的影响。最佳分离条件为:1%正庚烷(V/V),100mmol/LSDS,10%正丁醇(V/V)和8mmol/L磷酸盐-四硼酸钠缓冲溶液(pH7.30)。以氧氟沙星(OF)作内标,FQs标准水溶液和标准血清溶液的线性范围分别为1.2×10^-6~5.0×10^-4mol/L和2.0×10^-6~5.0×10^-4mol/L,检出限(S/N=3)均为9.7×10^-7mol/L。方法直接应用于滴眼液中环丙沙星(CPF)的测定,精密度和准确度高;应用于血液中加替沙星(GTF)的测定涉及固相萃取预处理样品,萃取平均回收率为90.6%,日内、日间精密度分别为3.3%和3.6%,结果满意。
A microemulsion electrokinetic capillary chromatographic (MEEKC) method has been developed for the simultaneous separation of seven fluoroquinolones (FQs) Using sodium dodeeylsulfate (SDS) as surfactant, an exhaustive study of the influence of buffer pH, phosphate concentration, SDS concentration, eo-surfaetant concentration, oil concentration and temperature has been carried out. Baseline separation of the seven FQs is achieved in a carrier electrolyte containing 1% (WV) heptane, 100 mmol/L SDS, 10 % (WV) 1-butanol, and 8-mmol/L phosphate-sodium tetraborate buffer at pH 7.30. Ofloxaxein (OF) was used as an internal standard. The linear concentration ranges of the method were 1.2 × 10^-6 - 5.0 × 10^ -4 mol/L and 2.0 × 10^-6 -5.0 ×10^-4 mol/L in aqueous standard solutions and serum, respectively. The detection limit ( S/N = 3 ) was 9.7 × 10 ^-7 mol/L. Direct measurements of eiprofloxaein (CPF) in pharmaceutical formulation were performed with high precision and accuracy. When the method was applied to serum samples combined with a solid-phase extraction treatment of samples using C18 cartridges, the mean extraction recovery was 90. 6%. The intra- and inter-day relative standard deviations (n = 6) were 3.3 % and 3.6%, respectively.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2008年第4期499-503,共5页
Chinese Journal of Analytical Chemistry
基金
广西自然科学基金(No.0640038)
肇庆市科技计划(No.10560)
肇庆学院自然科学基金(No.0737)资助项目
关键词
微乳液电动毛细管色谱
氟喹诺酮类药物
分离
Microemulsion electrokinetic capillary chromatography, fluoroquinolones, separation