摘要
目的：建立以HPLC荧光检测法测定人血浆中霉酚酸浓度的方法。方法：霉酚酸血浆样品经乙腈沉淀后取20μl直接进样,色谱柱为Hypersil BDS C18（250 mm ×4.6 mm,5μm）,流动相为乙腈-甲醇-0.2 mol·L-1磷酸氢二钾缓冲溶液（pH=9.0）（18∶2∶80）,柱温25℃,流速为1.0 ml·min-1,激发波长（Ex）为342 nm,发射波长（Em）为425 nm。结果：血浆内源性杂质和合并用药对测定无干扰,霉酚酸检测浓度在0.25~50.00mg·L-1范围内线性关系良好（r=0.9997）,定量下限为0.25 mg ·L-1；平均方法回收率为99.12%,平均提取回收率为93.27%；日内RSD小于2%,日间RSD小于6%。10例肾移植患者服用霉酚酸酯的剂量为0.5~1.75 g·d-1,血浆中霉酚酸浓度范围为0.43~21.58 mg·L-1。结论：本法快速、灵敏、准确、方便,可用于体内霉酚酸血药浓度分析及常规血药浓度监测。
Objective： To establish an HPLC-fluoremetry method for determination of the plasma concentration of mycophenolic acid （ MPA） in renal transplantation patients. Methods：The sample was subjected to precipitate proteins using acetonitrile, and the supernatant （20 μl） was used for the sample injection and determination on a Hypersil BDS C18 （250 mm × 4. 6 mm, 5 μm） column with temperature at 25℃. The mobile phase consisted of acetonitrile-methanol-0. 2 mol·L-1 dipotassium hydrogen phosphate buffer （pH=9. 0）（ 18∶2∶80）with the flow rate of 1. 0 ml·min-1. The excitation wavelength （Ex） was 342 nm and the emission wave-length （ Em） was 425 nm. Results：The endogenous plasma impurities and drug combinations had no interference with the determina-tion. The calibration curve was linear over the range of 0. 25-50. 00 mg·L-1（r=0. 999 7）, and the lower limit of quantification was 0. 25 mg·L-1 . The mean methodological recovery was 99. 12% and the mean extraction recovery was 93. 27%, the intra-day RSD was less than 2% and the inter-day RSD was less than 6%. Totally 10 cases of renal transplantation patients were with mycophenolate mofetil at the dose of 0. 5-1. 75 g·d-1 , and MPA in plasma was within the range of 0. 43-21. 58 mg·L-1 . Conclusion：The method is rapid, sensitive, accurate and convenient, which can be used in the quantitative determination of plasma concentration of MPA in re-nal transplantation patients.
出处
《中国药师》
CAS
2015年第5期744-747,共4页
China Pharmacist
关键词
高效液相色谱-荧光检测
肾移植
霉酚酸
血药浓度
HPLC-fluoremetry
Renal transplantation
Mycophenolic acid
Plasma concentration
