摘要
目的 建立反相高效液相色谱法测定犬血浆中磷酸川芎嗪 (TMPP)的浓度。方法 采用RP -HPLC ,使用Shim -packCLC-ODSC18柱 (15 0mm× 6 .0mm ,5 μm) ,流动相为甲醇 -水 (6 2∶38) ,流速 1.0ml·min-1,检测波长 2 79nm ,用卡马西平乙腈内标液沉淀蛋白后进样。结果 血浆中磷酸川芎嗪的最低检测浓度为 0 .0 5 μg·ml-1,分析时仅需血浆 10 0 μl。标准曲线线性范围为 0 .2～ 5 0 μg·ml-1,r =0 .9999;TMPP 3种浓度血浆样品的回收率为 99.4 %～ 10 4 .4 % ,日内RSD≤ 4 .5 2 % ,日间RSD≤7.4 6 %。结论 所用方法灵敏、可靠 。
OBJECTIVE To establish a sensitive and reliable RP HPLC method for the determination of tetramethylpyrazine phosphate (TMPP) in dog plasma. METHODS Concentrations of TMPP in plasma were measured by RP HPLC after pretreatment with carbamazepine (internal standard) acetonitrile solution to precipitate the protein. Seperation was achieved on a Shim pack CLC ODS C 18 column (150 mm×6.0 mm, 5 μm). The mobile phase consisted of methanol water (62∶38) at a flow rate of 1.0 ml·min -1 . TMPP was monitored at a wavelength of 279 nm.RESULTS The detection limit of TMPP in plasma was 0.05 μg·ml -1 , and only 100 μl of plasma was required for analysis. The calibration curve was linear in the range of 0.2-50 μg·ml -1 ,r=0.9999;The recoveries of TMPP from plasma at three different concentrations were between 99.4%～104.4%. The within day RSDs were less than 4.52%, and the between day RSDs were less than 7.46%.CONCLUSION The method could be applied for the pharmacokinetic research on TMPP and its preparations.
出处
《华西药学杂志》
CAS
CSCD
2003年第1期48-50,共3页
West China Journal of Pharmaceutical Sciences
