HPLC法测定泊沙康唑原料药中的有关物质

Determination of Related Substance in Posaconazole Raw Material by HPLC

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.