氧氟沙星分子烙印聚合物用于血清中6种氟喹诺酮的固相萃取  

Ofloxacin imprinted polymer applied to the solid-phase extraction of six fluoroquinolones from serum

作　　者：孙汉文[1] 刘广宇[1] 乔凤霞[1] 梁淑轩[1] 

机构地区：[1]河北大学化学与环境科学学院,河北省分析科学技术重点实验室,保定071002

出　　处：《药物分析杂志》2008年第6期848-852,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：教育部博士点学科基金项目:NO.20050075003

摘　　要：目的:制备氧氟沙星分子烙印聚合物,建立血清中氟喹诺酮药物的分子烙印固相萃取方法。方法:以甲基丙烯酸为功能单体,氧氟沙星为模板分子制备分子烙印聚合物。血清样品过分子烙印固相萃取柱,经水清洗和乙腈-三氟乙酸(99:1)洗脱后由高效液相色谱法分离。色谱柱为 Shimadzu VP ODS column(150 mm×4.6 mm,5μm).柱温30℃,流动相为乙腈-0.02 mol·L^(-1)四丁基溴化铵(用三氟乙酸调 pH=2.50)(9:91),流速1.0 mL·min^(-1),检测波长282 nm,进样20 μL。结果:制备的分子烙印聚合物对6种氟喹诺酮约物具有良好的吸附特性。结合位点的解离常数为 K_(d1)=1.04×10~4 mol·L^(-1),最大表观结合位点数 Q_(max.1)=79.10 μmol·g^(-1);低亲和力结合位点的解离常数为 K_(d2)=1.40×10^(-3)mol·L^(-1),最大表观结合位点数Q_(max.2)=276.79 μmol·g^(-1)。相邻分析物的分离度在1.49～2.06范围内。结论:所制备的分子烙印聚合物用于固相萃取-高效液相色谱可有效分离血清中6种氟喹诺酮类约物。Objective：To prepare ofloxacin molecular imprinted polymer （MIP） and develop a molecularly imprinted solid - phase extraction （MISPE） method for determination of six fluoroquinolones in serum. Methods ： The MIP was prepared using ofloxacin as template and methacrylic acid as functional monomer. Serum samples were prepared with molecularly imprinted solid - phase extraction column. All six kinds of fluoroquinolones in spiked goat serum samples were extracted with water and acetonitrile/trifluoracetic acid as washing and elution solution, respectively, followed by separation using high performance liquid chromatography. The chromatographic separation was performed on a Shimadzu VP- ODS column（ 150 mm ×4.6 mm,5 μm）at temperature of 30 ℃. The mobile phase,a mixture of acetonitrile - 0. 02 mol · L^-1 tetrabutl ammonium bromide （ adjusted with trifluoracetic acid to pH = 2.50） （9：91 ） ,was delivered at a flow rate of 1.0 mL·min^-1. The detection wavelength was 282 nm. Results：The MIP had a good adsorption speciality for six fluoroquinolones. For the higher affinity site,Kd1 = 1.04×10^-4mol· L^-1 ,and Qmax, 1 =79.10 μmol ·g^-1.For the lower affinity site, Kd2 =1.40×10^-3 mol·L^-1 ,and Qmax,2 =276.79 μmol·g^-1. Resolution of the neighbouring analytes was in the range of 1.49 -2.06. Conclusion：Use of the prepared MIP in solid phase extraction -high performance liquid chromatography can effectively separate six fluoro- quinolones in serum samples.

关 键 词：分子烙印(MIP) 固相萃取 氟喹诺酮 血清 

分 类 号：R917[医药卫生—药物分析学]