高效液相色谱法测定盐酸氨溴索注射液中2种杂质的含量

目的采用高效液相色谱法测定盐酸氨溴索注射液中2种有关物质的含量。方法采用辛烷基硅烷键合硅胶Kromasil 100-5C8柱(250 mm×4.6 mm,5μm),以磷酸二氢铵缓冲液(取磷酸氢二铵2 g,溶于800m L水中,用磷酸调p H值至4.0,再加水稀释成1 000 m L)-甲醇(45:55)为流动相,流速为1.0 m L·min-1,检测波长分别为238、250 nm,柱温:30℃。结果杂质B反-4-(6,8-二溴-1,2,3,4-四氢喹唑啉-3-基)环己醇和杂质E 2-氨基-3,5-二溴苯甲醛的检出限分别为9.39 ng、3.70 ng,定量限分别为18.78 ng、11.10ng;线性范围分别为0.376¹8.8μg·m L-1(r=0.999 9)、0.38618.8μg·m L-1(r=0.999 9)、0.386⁷.72μg·m L-1(r=0.999 8),平均加样回收率均在99.8%7.72μg·m L-1(r=0.999 8),平均加样回收率均在99.8%¹00.1%,RSD均<0.5%。结论该方法测定盐酸氨溴索注射液中的有关物质方法简便、准确、专属性强,可用于盐酸氨溴索注射液中有关物质的质量控制。

Content of 2 impurities in ambroxol hydrochloride injection by HPLC

Objective To establish an HPLC method to determine related substances in ambroxol hydrochloride injection. Methods Kromasil 100-5C8 column（250 mm×4.6 mm, 5 μm） was used. The mobile phase was ammonium dibasic phosphate buffer（p H = 4.0）-methanol（45 ：55） at 1.0 m L·min^- 1. The detection wavelength was 238 nm and 250 nm, the column temperature was 30 ℃. Results The minimum detection limit of impurity B trans-4-{（2-amino-3, 5-dibromophenyl） methyl] amino}-cyclohexanol and impurity E 2-amino-3, 5-two bromo benzaldehyde was 9.39 ng and 3.70 ng, respectively. The limits of quantification were 18.78 ng and 11.10 ng. The calibration curve of impurity B and impurity E had good linearity at 0.376- 18.8 μg·mL^- 1（r = 0.999 9） and 0.386- 7.72 μg·mL^- 1（r= 0.999 8）. The average recoveries of impurity B and impurity E were at 99.8%- 100.1%, with RSDs were less than 0.5%. Conclusion This method is easy to operate, reliable and highly sensitivite, which can be used to control the related substances in ambroxol hydrochloride injection.