摘要
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 mL·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0.376-18.8μg·mL^-1（r=0.999 9）、0.386-7.72μg·mL^-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。
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.
出处
《中南药学》
CAS
2014年第11期1136-1138,共3页
Central South Pharmacy
