高效液相色谱法同时测定己新替芬特罗糖浆中3种成分的应用价值

Application value of high-performance liquid chromatography in simultaneous determination of three ingredients in hexitalopram syrup

目的建立同时测定己新替芬特罗糖浆中盐酸溴己新、富马酸酮替芬与盐酸克仑特罗含量的方法。方法采用高效液相色谱法测定己新替芬特罗糖浆中盐酸溴己新、富马酸酮替芬与盐酸克仑特罗的含量。色谱柱为Waters Symmetry(4.6 mm×250 mm,5μm),流动相为乙腈-磷酸盐缓冲液(梯度洗脱),流速为1.0 ml/min,检测波长为244 nm,柱温为30℃。结果盐酸溴己新、富马酸酮替芬与盐酸克仑特罗的检测进样量线性范围分别为16.85~84.24μg/ml(r=0.9999)、4.100~24.60μg/ml(r=0.9999)、0.108~4.320μg/ml(r=0.9999);定量限分别为29.5 ng、20.5 ng、10.8 ng,检出限分别为8.4 ng、10.2 ng、2.6 ng;精密度、稳定性、重复性试验的RSD<2%;加样回收率分别为98.26%~99.24%(RSD=0.4%,n=6)、97.77%~99.76%(RSD=0.8%,n=6)、102.04%~103.98%(RSD=0.7%,n=6)。结论高效液相色谱法可用于同时测定己新替芬特罗糖浆中盐酸溴己新、富马酸酮替芬和盐酸克仑特罗的含量,其结果准确、精密度高。

Objective To establish a method for the contents determination of bromhexine hydrochloride,ketotifen fumarate and clenbuterol hydrochloride in hexitalopram syrup.Methods High-performance liquid chromatography was used for the content determination of bromhexine hydrochloride,ketotifen fumarate,clenbuterol hydrochloride.The column was Waters Symmetry（4.6 mm×250 mm,5 μm）,mobile phase was acetonitrile-phosphate buffer（gradient elution）,at a flow rate of 1.0 ml/min,detection wavelength was 244 nm,and the column temerpature was 30 ℃.Results The linear range of bromhexine hydrochloride,ketotifen fumarate,clenbuterol hydrochloride were 16.85-84.24 μg/ml（r=0.9999）,4.100-24.60 μg/ml（r=0.9999）,0.108-4.320 μg/ml（r=0.9999）;Limited of quantitation was respectively 29.5 ng、20.5 ng、10.8 ng,limited of detection was respectively 8.4 ng、10.2 ng、2.6 ng;RSDs of precision,stability and reproducibility tests were lower than 2%;Recovery were 98.26%-99.24%（RSD=0.4%,n=6）,97.77%-99.76%（RSD=0.8%,n=6）,102.04%-103.98%（RSD=0.7%,n=6） respectively.Conclusion The standard can effectively control the quality of bromhexine hydrochloride,ketotifen fumarate,clenbuterol hydrochloride in hexitalopram syrup,which has a higher accurate and precision.