HPLC法测定注射用盐酸哌甲酯中的有关物质

Determination of Related Substances in Methylphenidate Hydrochloride for Injection by HPLC

目的:建立测定注射用盐酸哌甲酯中有关物质的方法。方法:采用高效液相色谱法。色谱柱为Waters symmetry C_(18),流动相为甲醇-0.01 mol/L磷酸二氢钾溶液(60∶40,V/V),流速为1.0 m L/min,检测波长为210 nm,柱温为35℃,进样量为10μL。结果:杂质A、杂质B检测质量浓度线性范围均为0.02~3.0μg/m L(r均为0.999 8);定量限分别为0.2、0.6 ng,检测限分别为0.06、0.2 ng;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为98.2%~100.0%(RSD=0.56%,n=9)、98.0%~100.3%(RSD=0.70%,n=9)。结论:该方法操作简便、结果准确,适用于注射用盐酸哌甲酯中有关物质的测定。

OBJECTIVE： To establish a method for the determination of related substances in Methylphenidate hydrochloride for injection. METHODS： HPLC method was adopted. The determination was performed on Waters symmetry C18 column with mobile phase consisted of methanol-0.01 mol/L potassium dihydrogen phosphate solution （60：40, V/V） at the flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm, the column temperature was 35 -C and sample size was 10 pL. RESULTS： The linear range of impurity A and B were 0.02-3.0 μg/mL （r=0.999 8）. The limits of quantitation were 0.2, 0.6 ng, and the limits of detection were 0.06, 0.2 ng, respectively. RSDs of precision, stability and reproducibility were all lower than 2.0% ; recoveries were 98.2%-100.0% （RSD=0.56% ,n-=-9）, 98.0%-100.3% （RSD=0.70% ,n=9）, respectively. CONCLUSIONS： The method is simple, accurate and suitable for the determination of related substance in Methylphenidate hydrochloride for injection.