摘要
目的:建立测定泊沙康唑原料药中有关物质的方法。方法:采用高效液相色谱法。色谱柱为Zorbax Eclipse Plus C_(18),流动相为0.05 mol/L醋酸铵溶液(加醋酸调节pH为4.0)-乙腈(梯度洗脱),流速为1.0 mL/min,检测波长为262 nm,柱温为30℃,进样量为20μL。结果:中间体Ⅰ检测质量浓度线性范围为0.05~5.0μg/mL(r=0.999 9);定量限为0.05μg/mL,检测限为0.013μg/mL;精密度、稳定性、重复性试验的RSD<2.0%;回收率为98.00%~101.69%(RSD=1.22%,n=9)。结论:该方法操作简便、结果准确,适用于泊沙康唑原料药中有关物质的测定。
BJECTIVE: To establish a method for the determination of related substance in posaconazole raw material. METHODS: HPLC method was adopted. The separation was performed on Zorbax Eclipse Plus C18 column with mobile phase consisted of 0.05 mol/L ammonium acetate solution (pH adjusted to 4.0 using acetic acid)-acetonitrile (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength was set at 262 nm, and the column temperature was 30 ℃. The sample size was 20 μL. RESULTS: The linear range of intermediateⅠwas 0.05-5.0 μg/mL (r=0.999 9); the limit of quantitation was 0.05 μg/mL, the limit of detection was 0.013 μg/mL; RSDs of precision test, stability test and repeatability test were lower than 2.0%; the recoveries was 98.00%-101.69%(RSD=1.22%,n=9). CONCLUSIONS: The method is simple, accurate and suitable for the determination of related substance in posaconazole raw material.
出处
《中国药房》
CAS
北大核心
2017年第36期5157-5159,共3页
China Pharmacy