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固相萃取-反相HPLC法同时快速测定血浆中4种氟喹诺酮类药物
Quick separation and determination of four fluoroquinolones in human plasma by SPE and RP-HPLC
【摘要】 目的建立同时快速测定人血浆中4种氟喹诺酮类药物(氟罗沙星、左氧氟沙星、诺氟沙星和环丙沙星)的方法。方法采用C18固相萃取小柱萃取血浆中的4种氟喹诺酮类药物。色谱柱为ODS-BP柱(5μm,250mm×4.6mm),流动相为含1.31g/LL-异亮氨酸和0.80g/L CuSO4的水溶液-甲醇(80∶20,V∶V),激发波长为280nm,发射波长为504nm,流速为0.8ml/min。结果4种氟喹诺酮类药物可良好分离,分离度达到1.5以上。4种药物的线性范围均是0.1-20μg/ml,r均大于0.9975,氟罗沙星、左氧氟沙星、诺氟沙星和环丙沙星的最小检测限依次分别为50ng/ml、1ng/ml、100ng/ml、100ng/ml,萃取回收率均高于87.97%,方法回收率均在95.40%与101.82%之间,日内RSD均小于3.7%,日间RSD均小于1.5%。结论固相萃取-反相HPLC法简便,灵敏度高,准确度高,精密度好,可用于氟喹诺酮类药物的快速测定。
【Abstract】 Objective To establish a better method for quickly separating and determining four fluoroquinolones(FLX,LVFX,NFLX,CPFX)in human serum by SPE and RP-HPLC. Methods The four fluoroquinolones in human serum were extracted by SPE with C18 SPE column,and the quantities of the four fluoroquinolones were separated and determined by RP-HPLC.The chromatography column was a ODS-BP column(5 μm,250 mm×4.6 mm).The mobile phase was made up of the water solution(1.31 g/L isoleucine and 0.80 g/L CuSO4)and methanol(80∶20,V∶V).The excitation and emission wavelengths were 280 nm and 504 nm.The flow rate was 0.8 ml/min. Results The four fluoroquinolones were successfully separated and all the resolutions were above 1.5.All the linear ranges of them were 0.1-20 μg/ml,and r values were all above 0.997 5.The detection limits were 50 ng/ml,1 ng/ml,100 ng/ml,100 ng/ml(S∶N=3∶1),respectively.The mean extraction recoveries were all above 87.97%,and the mean method recoveries of them were 95.40%-101.82%.All the within-day RSDs were below 3.7%,and all the between-day RSDs were below 1.5%. Conclusion The methods are simple,rapid,sensitive,accurate and precise for rapid determining fluoroquinolone.
【Key words】 solid phase extraction; fleroxacin; levofloxacin; norfloxacin; ciprofloxacin; drug abuse;
- 【文献出处】 山西医科大学学报 ,Journal of Shanxi Medical University , 编辑部邮箱 ,2008年11期
- 【分类号】R96
- 【被引频次】5
- 【下载频次】154