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建立并评价了一种简单灵敏的方法测定狗血浆中PZS的含量.该方法利用HPLC-FLD结合乙醚萃取的前处理方法,采用C18色谱柱(150mm×4.6mm,5μm),流动相为30%乙腈和70%乙酸-乙酸钠缓冲液(pH=3.6),荧光检测器的激发波长为258nm,发射波长为387nm,在流动相流速为1.0mL/min时,其PZS和内标物的保留时间分别为4.4和5.8min.标准曲线在1.0～1000.0ng/mL的浓度范围内呈线性相关(r2>0.998),检出限为0.4ng/mL,标准曲线的日间变异系数低于5.0%,准确度在92.7%～104.2%范围内.在3d的分析质量控制研究中,日内和日间精密度均小于10%,准确度为95.9%～112.7%.该方法成功应用于一种新的口服制剂(PZS-磺丁基醚-β-环糊精包合物)的临床前期药代动力学评价,结果表明:该新型的包合药物具有缓释PZS的功效,且其相对生物利用率为105.0%.
A simple and sensitive method for the determination of PZS in dog plasma was established and evaluated.Using HPLC-FLD combined with ether extraction, a C18 column (150 mm × 4.6 mm, 5 μm) with a mobile phase of 30% Acetonitrile and 70% acetic acid-sodium acetate buffer (pH = 3.6). The fluorescence detector has an excitation wavelength of 258 nm and an emission wavelength of 387 nm. When the mobile phase flow rate is 1.0 mL / min, the retention time of PZS and internal standard (R2> 0.998), the detection limit was 0.4ng / mL, the coefficient of variation of the standard curve was lower than 5.0% The accuracy was between 92.7% and 104.2% .In the analysis of quality control of 3d, the intra-day and inter-day precision were less than 10% and the accuracy was 95.9% ~ 112.7% .The method was successfully applied to a new oral (PZS-sulfobutylether-β-cyclodextrin inclusion complex), the results showed that the new inclusion compound has the efficacy of sustained release PZS, and its relative bioavailability was 105.0%.