论文部分内容阅读
建立以2,3,4,6-四乙酰基--βD-吡喃葡萄糖基异硫氰酸酯(GITC)为手性衍生化试剂测定血浆中普萘洛尔对映体浓度的反相高效液相色谱方法。血浆样品经甲醇除蛋白。采用C18色谱柱(4.6 mm×250 mm,5μm,Bnentnach),流动相为甲醇-20 mmol/LKH2PO4的水溶液(75∶25);流速1 mL/min;检测波长220 nm。结果:S(-)-普萘洛尔和R(+)-普萘洛尔检测浓度在1.00~277.78μg/mL浓度范围内与色谱峰面积有良好的线性关系。日内、日间精密度均小于5%,回收率分别为98.95%和105.76%,RSD均小于7.13%。结论:本方法灵敏度高,重现性可用于血浆中普萘洛尔对映体的分离测定。
To establish a reversed-phase and high-efficiency method for the determination of enantiomer concentrations of propranolol in plasma by 2,3,4,6-tetraacetyl-βD-glucopyranosyl isothiocyanate (GITC) as a chiral derivatization reagent Liquid chromatography method. Plasma samples were denitrified with methanol. C18 column (4.6 mm × 250 mm, 5 μm, Bnentnach) was used. The mobile phase consisted of methanol-20 mmol / L KH 2 PO 4 in water (75:25), the flow rate was 1 mL / min and the detection wavelength was 220 nm. Results: The calibration curve of S (-) - propranolol and R (+) - propranolol showed a good linear relationship with the chromatographic peak area in the range of 1.00-277.78 μg / mL. The intra-day and inter-day precision were less than 5%, the recovery rates were 98.95% and 105.76%, respectively, with RSDs less than 7.13%. Conclusion: The method is sensitive and reproducible for the separation and determination of propranolol enantiomers in plasma.