HPLC法测定尼鲁米特原料药的含量和杂质

目的:建立测定尼鲁米特原料药含量和杂质的方法。方法:采用高效液相色谱法。尼鲁米特和杂质(总杂质、杂质Ⅰ)的流动相体系分别采用乙腈-磷酸二氢钾溶液(pH 7.5)梯度洗脱和等度洗脱,二极管阵列检测波长分别为267、230 nm,其余条件均相同,色谱柱为WondaSil C18-WR,柱温为30℃,进样量为10μl。结果:尼鲁米特、杂质Ⅰ的检测质量浓度线性范围分别为0.1¹.25 mg/ml、0.641.25 mg/ml、0.64⁶.40μg/m(lr=0.999 6、0.999 9);平均回收率分别为94.2%(RSD=0.57%,n=2)、98.6%(RSD=2.1%,n=2)。杂质Ⅰ的限度应控制在0.2%以下,总杂质不得大于2.0%。结论:本方法快速、简便、专属性强,能有效控制尼鲁米特原料药质量。

Content Determination and Related Impurities in Nilutamide Raw Material by HPLC

OBJECTIVE： To establish the method for the content determination of nilutamide and impurities. METHODS： HPLC method was adopted. WondaSil C18-WR column was used with mobile phase consisted of acetonitrile-potassium dihydrogen phosphate solution （adjust pH to 7.5, gradient elution and isocratic elution）, along with a diode array detector （DAD） to control nilutamide and impurity. The detection wavelength was set at 267 nm and 230 nm. Other detection conditions were same to each other. The column temperature was 30 ℃, and sample size was 10 txl. RESULTS： The linear range of nilutamide and impurity I were 0.1-1.25 mg/ml （r=0.999 6） and 0.64-6.40 μg/ml （0.999 9） ; average recoveries were 94.2% （RSD=0.57%, n=2） and 98.6% （RSD=2.1%, n=2）. The impurity I was not more than 0.2%, and total impurity was less than 2.0%. CONCLUSIONS： The method is rapid, simple and specific, and suitable for the quality control of nilutamide raw material.