高效液相色谱法测定盐酸氨溴索注射液中有关物质含量

目的：建立盐酸氨溴索注射液中有关物质定量的高效液相色谱（HPLC）法。方法采用高效液相色谱双波长法测定含量。色谱柱为XB-C18柱（Agilent Zorbax 250 mm ×4.6 mm，5μm），0.01 mol/L磷酸氢二铵溶液（用磷酸调节pH至7.0）-乙腈（42：58）为流动相，检测波长为250 nm（检测盐酸氨溴索、杂质B与其他杂质）与238 nm（检测杂质E），柱温为40℃，流速为1.0 mL/min，进样量为20μL。结果杂质A进样量在0.020~20.02μg范围内与峰面积呈良好线性关系（ r=0.9999）；杂质B进样量在0.0602~20.08μg范围内与峰面积呈良好线性关系（ r=0.9996），平均回收率为99.6%（ n=6）；杂质D进样量在0.0607~20.22μg范围内与峰面积呈良好线性关系（ r=0.9991）；杂质 E 进样量在0.061~20.16μg范围内与峰面积呈良好线性关系（ r=0.9993），平均回收率为99.8%（ n=6）；盐酸氨溴索（λ=250 nm和λ=238 nm）进样量在0.060~20.16μg范围内与峰面积呈良好线性关系（ r=0.9997，r=0.9995）。结论该方法定量准确可靠，方法简便、操作简单、灵敏度高，适用于盐酸氨溴索注射液中有关物质质量控制。

HPLC Determination of Related Substance Content in Ambroxol Hydrochloride Injection

Objective To establish a method for determining the related substance content in Ambroxol Hydrochloride Injection. Methods The HPLC method was adopted for conducting the dual wavelength determination of the content of the related substances in Ambroxol Hydrochloride Injection. The XB-C18 column （ Agilent Zorbax 250 mm × 4. 6mm, 5 μm ） was adopted with 0. 01 mol/L diammonium phosphate solution （ adjusting pH to 7. 0 with phosphoric acid ） -acetonitrile （ 42 ：58 ） as the mobile phase, the detection wavelength of 250 nm （ testing ambroxol hydrochloride, impurities B and other impurities ） and 238 nm （ testing impurity E ） as the mobile phase; the column temperature was 40℃;the flow rate was 1. 0 mL/min;the sample size was 20 μL. Results The impurity A sample size in the range of 0. 020-20. 02μg had good linear relationship （ r=0. 999 9 ）;the impurity B sample size in the range of 0. 602-20. 08μg had good linear relationship（ r=0. 999 6）, the average recovery rate was 99. 6%（ n=6）;the impurity D sample size in the range of 0. 060 7-20. 22μg had good linear relationship （ r=0. 999 1 ）;the impurity E sample size in the range of 0. 061-20. 16μg had good linear re-lationship （ r=0. 999 3 ） , the average recovery rate was 99. 8% （ n=6 ）;the ambroxol hydrochloride （ 250 nm, 238 nm ） sample size in the range of 0. 060-20. 16μg had good linear relationship （ r=0. 999 7, r=0. 999 5 ） . Conclusion This method is accurate and reliable in quantitation, simple and convenient to operate, highly sensitive and suitable for the quality control of related substances in Ambroxol Hy-drochloride Injection.