固相萃取高效液相色谱法测定人血浆中头孢泊肟浓度  被引量:4

Determination of cefpodoxime concentration in plasma by solid-phase extraction and HPLC

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作  者:吴丽花[1] 申屠建中[1] 章霞[1] 陈志根[1] 史美甫[1] 

机构地区:[1]浙江大学医学院附属第一医院,浙江杭州310003

出  处:《中国医院药学杂志》2003年第9期513-514,共2页Chinese Journal of Hospital Pharmacy

摘  要:目的 :建立人血浆中头孢泊肟的高效液相色谱测定法。方法 :采用固相萃取法预处理血浆样品 ,分析柱为M N Necleosil 10 0 5C18柱 (15 0mm× 4 .6mm ,5 μm) ,流动相为pH 3.8的 0 .0 5mol·L-1醋酸缓冲液 甲醇 (82∶18) ,流速为 1mL·min-1,检测波长为 2 34nm ,柱温为 39℃ ,按内标法定量。结果 :头孢泊肟与内标固定物的保留时间为 7.77min和 8.93min ;头孢泊肟血药浓度线性范围为 0 .0 5~ 5 .0mg·L-1(r =0 .9999) ,最低检测浓度为 0 .0 2 5mg·L-1(S/N≥ 3) ,萃取回收率在 84 %~ 95 % (n =5 ) ,分析方法回收率在 98%~ 10 6 % (n =5 ) ,日内和日间RSD分别为 2 .5 %~ 6 .6 %和 1.8%~ 4 .2 % (n =5 )。结论 :本法操作便捷 ,灵敏度和精密度高 ,重现性好 。OBJECTIVE To establish an HPLC method for determination of cefpodoxime in human plasma. METHODS Plasma samples were pretreated by solid phase extraction. Cefpodoxime and cefuroxime (internal standard) were separated on M N Necleosil 100 5 C 18 column( 150 mm × 4.6 mm , 5 μm )at 39 ℃ with 0.05 mol ·L -1 acetate buffer of pH 3.8 methanol(82∶18)as mobile phase at a flow rate of 1 mL ·min -1 , and monitored at 234 nm . RESULTS Cefpodoxime and cefuroxime was eluted at about 7.77 min and 8.93 min after injection,respectively. Calibration curve in human plasma was linear ( r = 0.9999 ) in the range of 0.05 to 5.0 mg ·L -1 , the detection limit was 0.025 mg · L -1 (S/N≥3 ),the extraction recovery was 84%~95%( n =5),the analytical recovery was 98%~106%( n =5),the within day RSD and between day RSD were 2.5% ~ 6.6% and 1.8% ~ 4.2% ( n =5),respectively.CONCLUSIONS The method is simple,sensitive and reproducible,and is suitable for the pharmacokinetic study of cefpodoxime.

关 键 词:头孢泊肟 固相萃取 高效液相色谱法 人血浆 血药浓度 测定 

分 类 号:R969.2[医药卫生—药理学] R978.1[医药卫生—药学]

 

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