高效液相色谱法测定硫酸沙丁胺醇有关物质的含量

HPLC method was used to determine the content of albuterol sulfate

目的建立硫酸沙丁胺醇原料药有关物质的检测方法。方法采用高效液相色谱(HPLC)法测定。色谱柱为Hypersil Gold C8柱(250 mm×4.6 mm,3μm),流动相A为3.45 g一水合磷酸二氢钠用900 m L 0.05%的三乙酸胺溶液溶解,以稀磷酸调节pH至3.0之后用0.05%的三乙酸胺溶液定容至1 000 mL;流动相B为甲醇∶乙腈(体积比20∶80),进行梯度洗脱;流速为1.0mL/min,检测波长为273 nm,柱温为25℃。结果在该色谱条件下,硫酸沙丁胺醇及杂质A、B、C、D、E、F、G、K、M、O、L、Q、I、J均能有效分离,分离度均大于1.5;并且硫酸沙丁胺醇及杂质C、D、F、M、O在0.45~18.0μg/mL内质量浓度与峰面积线性关系良好,回收率分别为杂质C为99.1%,RSD为2.6%(n=9);杂质D为99.3%,RSD为2.1%(n=9);杂质F为100.1%,RSD为2.5%(n=9);杂质M为100.5%,RSD为1.7%(n=9);杂质O为100.2%,RSD为1.9%(n=9)。结论该方法专属性强,适用于硫酸沙丁胺醇原料药有关物质检测。

Objective To establish a method for detecting substances related to albuterol sulphate.Methods HPLC method was used for determination.Chromatographic column for Hypersil Gold C8 column(250 mm × 4.6 mm,3 microns),A 3.45 g mobile phase monohydrate sodium dihydrogen phosphate,with 900 mL.Three acetic acid amine solution of 0.05%,with A dilute phosphoric acid to adjust pH to 3.0 after three acetic acid with 0.05% of the amine solution constant volume to 1 000 mL;the flow phase B is methanol∶acetonitrile(volume ratio 20∶80),gradient elution;the velocity is 1.0 mL/min,the detection wavelength is 273 nm,and the column temperature is 25.Results In this chromatographic condition,salbutamol sulfate and impurities A,B,C,D,E,F,G,K,M,O,L,Q,I,J can be effectively separated,and the chromatographic resolution is greater than 1.5.In addition,salbutamol and impurities C,D,F,M and O are in good linear relationship with the peak area in 0.45%-18.0.The recovery rate of impurities C was99.1%,and the RSD was 2.6 %(n=9).The recovery rate of impurities D is 99.3%,and RSD is 2.1%(n=9).The recovery rate of impurities F was 100.1%,RSD was 2.5%(n=9).The recovery rate of impurities M was 100.5%,and RSD was 1.7%(n=9).The recovery rate of impurities O was 100.2% and RSD was 1.9 %(n=9).Conclusion This method has strong specificity and is suitable for the detection of substances related to albuterol sulfate.