A sensitive, selective and simple method using a precipitation of protein with 10% perchloric acid, followed by high-performance liquid chromatography (HPLC) with fluorescence detection was developed for the determination of itopride hydrochloride in human plasma, using levofloxacin as the internal standard (IS). Chromatographic separation was obtained within 7.0 min using a reverse phase Hypersil BDS C(18) (250 mm x 4.6 mm, 5 microm) column and an isocratic mobile phase, constituting of a mixture of 0.1 mol/l ammonium acetate-methanol (30:70, v/v) flowing at 1.1 ml/min. The excitation and emission wavelengths were set at 304 and 344 nm, respectively. The method was validated over the concentration range of 5 ng/ml to 1000.0 ng/ml. The lower limit of quantitation (LLOQ) was 5 ng/ml. The extractive recovery of itopride hydrochloride from the biological matrix was more than 80.77%. The intra-day accuracy of the drug containing serum samples was more than 82.94% with a precision of 2.81-4.37%. The inter-day accuracy was 82.91% or more, with a precision of 6.89-9.54%. The limit we have used (70-143%) is based on the local regulatory authority (SFDA). The developed method was validated and successfully applied to bioequivalence studies of itopride hydrochloride in healthy male volunteers.

译文

:以左氧氟沙星为内标,开发了一种灵敏,选择性,简单的方法,该方法使用10%高氯酸沉淀蛋白质,然后进行高效液相色谱(HPLC)和荧光检测,用于测定人血浆中的盐酸伊托必利(是)。使用反相Hypersil BDS C(18)(250 mm x 4.6 mm,5 microm)色谱柱和等度流动相,在7.0分钟内完成色谱分离,该流动相由0.1 mol / l乙酸铵-甲醇(30: 70,v / v)以1.1ml / min流动。激发和发射波长分别设置为304和344 nm。该方法在5 ng / ml至1000.0 ng / ml的浓度范围内得到验证。定量下限(LLOQ)为5 ng / ml。从生物基质中提取盐酸伊托必利的回收率超过80.77%。含药物血清样品的日内准确度超过82.94%,准确度为2.81-4.37%。日间精度为82.91%或更高,精度为6.89-9.54%。我们使用的限制(70-143%)基于当地监管机构(SFDA)。验证了所开发的方法,并将其成功应用于健康男性志愿者中盐酸伊托必利的生物等效性研究。

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