固相萃取高效液相色谱法测定血浆中亚甲蓝含量  

Determination of methylene blue in blood by HPLC and SPE

作　　者：王若燕[1] 周晓萍[1] 杜赛 

机构地区：[1]浙江省绍兴市疾病预防控制中心,浙江绍兴312000

出　　处：《中国卫生检验杂志》2008年第10期2012-2013,共2页Chinese Journal of Health Laboratory Technology

摘　　要：目的：建立血浆中亚甲蓝检测的高效液相色谱方法。方法：采用Waters OASIS HLB固相萃取小柱对血浆样品中残留的亚甲蓝进行萃取富集,采用高效液相色谱法SUNFIRE C18柱（5μm 4.6×250 mm）;流动相：水/乙腈/乙酸钠/乙酸/EDTA：750 ml/250 ml/6.5 g/8 ml/54 mg;流速：1.0 ml/min;柱温：25℃;二极管阵列检测器：293 nm进行分离测定,外标法定量。结果：在0.05～1.5μmol/L浓度范围,其线性关系良好,Y=342950X＋4298,相关系数（r）≥0.999。RSD为2.1%～3.8%,回收率可达到95%～99%。最低检测浓度为0.04μmol/L。结论：该方法具有准确、灵敏、快速、简便等特点,能够用于经亚甲蓝处理的血浆样品的检测。Objective：To establish the method of high-performance liquid chromatography for the determination of methylene blue in blood plasma.Methods：First the methylene blue in blood plasma was extracted and collected by the waters OASIS HLB solid-phase extraction little column,then the samples were separated on Sunfire C18（250 mm×4.6 mm×5 μm） and determined by PDA at 293 nm.Then the external standard method was used to verify quantify.The mobile phase was H2O（750 ml）/CH3CN（250 ml）/CH3COONa（6.5 g）/CH3COOH（8 ml）/EDTA（54 mg）.The flow rate was 1.0 ml/min,and the column temperature was controlled at 30℃.Results：The equation of line was Y=342950X＋4298,r≧0.999,linear range was 0.05～1.5 μmol/L.Its recovery rate was 95%～99%,and relative standard deviation rate was 2.1%～3.8%.Its monitoring limit was 0.05 mg/kg.Conclusion：This methods is accurate,sensitive,simple and convenient.It can be applied to determine the methylene blue in blood plasma.

关 键 词：固相萃取 高效液相色谱 亚甲蓝 

分 类 号：O657.72[理学—分析化学]