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目的:建立微量血浆中酒石酸唑吡坦的含量测定方法。方法:取大鼠,ig酒石酸唑吡坦溶液3 mg/kg,给药后取血0.2 ml,分离后取血浆50μl经甲醇沉淀蛋白,取上清液采用高效液相色谱-荧光法测定,以外标法进行定量。色谱柱为Agilent HC-C18,流动相为0.03 mol/L磷酸二氢钾溶液(含0.2%三乙胺)-甲醇(33∶67,V/V),流速为1.0 ml/min,激发波长为254 nm,发射波长为390nm,进样量为20μl。结果:酒石酸唑吡坦检测质量浓度的线性范围为2~200μg/L(r=0.999 7),定量下限为2μg/L;方法回收率为(96.96±1.35)%~(105.0±5.36)%(RSD为2.20%~4.88%,n=5);提取回收率为(79.72±0.01)%~(80.77±0.02)%(RSD为1.34%~3.90%,n=5);日内RSD为1.40%~5.10%,日间RSD为3.22%~9.25%(n=5)。结论:本法简便、灵敏,可用于微量血浆中唑吡坦的含量测定。
Objective: To establish a method for the determination of zolpidem tartrate in blood plasma. Methods: The rat and ig Zolpidem tartrate solution 3 mg / kg, blood 0.2 ml after administration, the plasma was separated 50μl after precipitation of the protein by methanol, the supernatant was determined by high performance liquid chromatography - fluorescence spectrometry Standard method for quantitative. The column was Agilent HC-C18 with a mobile phase of 0.03 mol / L potassium dihydrogen phosphate (containing 0.2% triethylamine) -methanol (33:67, V / V) at a flow rate of 1.0 ml / min. 254 nm, emission wavelength of 390nm, injection volume of 20μl. Results: The linear range of the concentration of Zolpidem tartrate was 2 ~ 200μg / L (r = 0.999 7) and the limit of quantification was 2μg / L. The recovery rate was (96.96 ± 1.35)% ~ (105.0 ± 5.36)% RSD was 2.20% -4.88%, n = 5). The recovery was (79.72 ± 0.01)% ~ (80.77 ± 0.02)% (RSD 1.34% -3.90%, n = 5) 5.10%, daytime RSD was 3.22% ~ 9.25% (n = 5). Conclusion: This method is simple, sensitive and can be used for the determination of zolpidem in trace plasma.