目的 建立鹽酸烏拉地爾原料藥中有關(guān)物質(zhì)的HPLC檢測方法。方法 采用Agilent XDB C₁₈色譜柱（250 mm×4.6 mm ，5 μm），以0.05 mol·L^-1磷酸二氫銨溶液（含0.02%三乙胺，磷酸調(diào)pH值至6.0）為流動相A，乙腈為流動相B，梯度洗脫；體積流量為1.0 mL·min^-1，柱溫為30℃，檢測波長為270、236 nm，進樣量為10 μL。進行方法專屬性、穩(wěn)定性、檢測限與定量限、線性關(guān)系、精密度、耐用性考察。應(yīng)用所建立的方法進行3批鹽酸烏拉地爾原料藥樣品檢測。結(jié)果 鹽酸烏拉地爾與相鄰雜質(zhì)之間、各雜質(zhì)之間的色譜峰均分離良好；各個組分的檢測限和定量限分別為0.059 7～0.090 0 μg·mL^-1、0.198 9～0.299 9 μg·mL^-1。各組分在相應(yīng)濃度范圍內(nèi)均有良好的線性關(guān)系，r均在0.999 8～1.000 0。加樣回收率均在92.2%～103.2%，RSD均≤5.37%。3批鹽酸烏拉地爾原料藥樣品檢測結(jié)果顯示，已知雜質(zhì)質(zhì)量分數(shù)均小于0.15%、最大未知單雜均小于0.10%，雜質(zhì)總質(zhì)量分數(shù)小于0.50%。結(jié)論 經(jīng)方法學(xué)驗證，所建立方法靈敏、高效、專屬性強、準確度高，可用于鹽酸烏拉地爾原料藥有關(guān)物質(zhì)的測定。

Objective To establish an HPLC method for the determination of related substances in urapidil hydrochloride. Method Agilent XDB C₁₈ (250 mm×4.6 mm, 5 μm) was chosen for analysis. Gradient elution was used to determine the related substances of urapidil hydrochloride with 0.05 mol·L^-1 ammonium dihydrogen phosphate (containing 0.02% triethylamine, and pH adjusted to 6.0 with phosphoric acid), and acetonitrile as mobile phase B. The flow rate was 1.0 mL·min^-1 and the column temperature was 30℃. The detection wavelengths were 270, 236 nm, and the sample injection volume was 10 μL. The specificity, stability, limit of detection and limit of quantification, linear relationship, precision and durability of the method were investigated. Three batches of urapidil hydrochloride API samples were detected by the established method. Results The resolution between urapidil and all other impurities were good. The limits of detection of urapidil hydrochloride and impurities were 0.059 7-0.090 0 μg·mL^-1 and the limits of quantitation of them were 0.198 9-0.299 9 μg·mL^-1. All known impurities had good linearity in appropriate concentration ranges and the correlation coefficients were all in the range of 0.999 8-1.000 0. The average recoveries of all known impurities were in the range of 92.2%-103.2%, with RSD of less 5.37%. The determination results of three batches of urapidil hydrochloride samples showed that the known impurities and the maximum unknown impurity were less than 0.10% and the total impurities were less than 0.5%. Conclusion The method was simple, rapid and accurate, which can be used to control the quality of urapidil hydrochloride.

R932