摘要
目的:建立二维液相色谱(2D-LC/UV)法测定血清中苯妥英的方法,以提高治疗药物监测水平。方法:一维色谱柱为Aston SC2柱(4.6 mm×25 mm,5μm),流动相为VCV-1D移动相,流速0.7 mL·min^(-1);二维色谱柱为Aston SCB柱(4.6mm×100 mm,5μm),流动相为BPI-1碱性流动相∶API-1酸性流动相∶MPI-1移动相=11∶37∶52(V∶V∶V),流速1.2mL·min^(-1);捕集柱为Aston SH柱(3.0 mm×10 mm,5μm),流动相为纯水;柱温40℃;紫外检测波长240 nm;外标法计算结果。结果:苯妥英在1.54~49.30μg·mL^(-1)范围内线性关系良好,r=0.999 9,可在7 min内完整出峰;方法回收率高于94%;日内、日间的精密度RSD均小于3.53%;稳定性试验RSD均小于5%。采集30例口服苯妥英钠患者血清样本进行检测,结果显示不在治疗窗内的患者占总人数的36.7%。结论:本方法自动化程度高、稳定性良好、检测快速准确,适用于苯妥英的血药浓度监测。
Objective： To establish a method for the determination of phenytoin in serum by two-dimensional liquid chromatography （2D-LC/UV） and improve the monitoring level of therapeutic drugs. Methods： The chromatographic column of one-dimensional liquid chromatography, trap column and two-dimensional liquid chromatography were Aston SC2 （4.6 mm × 25 mm, 5 μm）, Aston SH （3.0 mm × 10 mm, 5 μm） and Aston SCB （4.6 mm × 100 mm, 5 μm） respectively. The mobile phase of one-dimensional liquid chromatography, trap column and two-dimensional liquid chromatography were VCV-1D （flow rate was 0.7 mL·min^-1）, pure water and mixed mobile phase （BPI-1 basic mobile phase ： API-1 acidic mobile phase ： MPI-1 mobile phase = 11 ： 37 ： 52, fow rate was 1.2 mL·min-1） respectively. The column temperature was maintained at 40 ℃. The UV absorption wave length was set at 240 nm. Results were calculated by external standard method. Results： Phenytoin showed good linearity at the range of 1.54 – 49.3 μg·mL-1 （r = 0.999 9）. Phenytoin had a complete chromatographic peak within 7 minutes. The recovery rate was higher than 94%. RSDs of intra-day and inter-day precision were all less than 3.53%. RSD of the stability test was less than 5%. Results of serum samples from 30 patients taking oral phenytoin sodium showed that the serum concentration of phenytoin of 36.7% of the patients were out of the treatment window. Conclusion： This method was fast and accurate. It has high automation, good stability, which was suitable for the serum concentration monitoring of phenytoin.
作者
院江丽
张寒娟
袁冬冬
YUAN Jiang-li;ZHANG Han-juan;YUAN Dong-dong(Department of Pharmacy,the 7th People＇s Hospital of Zhengzhou City,Zhengzhou 450016,China;College of Pharmacy,Xinxiang Medical University,Xinxiang 453003,China)
出处
《中国药物应用与监测》
CAS
2018年第5期277-280,共4页
Chinese Journal of Drug Application and Monitoring
基金
常州四药临床药学科研基金项目(CZSYJJ15006)
关键词
二维液相色谱
苯妥英
血药浓度监测
Two-dimensional liquid chromatography
Phenytoin
Therapeutic drug monitoring
