RP-HPLC法测定雾化温度对吸入用布地奈德混悬液稳定性的影响

The influence of atomization temperature on the stability of inhaled Budesonide suspension by RP-HPLC determination

目的:建立雾化温度对吸入用布地奈德混悬液稳定性影响的测定方法。方法:采用反相高效液相色谱(RP-HPLC)法,以Gemini C18色谱柱(4.6 mm×250 mm,5 m)为分离柱,以甲醇+水82∶18(V/V)体积比为流动相,流速为1.0 ml/min,检测波长为244 nm,柱温约为25℃,测定雾化温度对吸入用布地奈德混悬液稳定性的影响。结果:布地奈德的保留时间约为6 min,布地奈德与其他组峰的分离度>1.5;方法精密度试验RSD为0.46%;供试品溶液在24 h内稳定。布地奈德在浓度0.01~0.15 mg/ml范围内与峰面积呈现良好的线性关系,回归方程为:A=5×107 c+20336(r=0.9999)。不同批次样品测量平均回收率为96.35%(RSD=1.01%,n=3)。超声雾化仪药杯底部中心点最高温度≤46℃,供试品溶液在80℃以内稳定。结论:RP-HPLC法测定吸入用布地奈德混悬液的含量,其精密度好、准确度高,布地奈德在雾化过程中能够保持稳定,不受温度变化的影响。

Objective:To establish a determination method for the influence of atomization temperature on the stability of inhaled Budesonide suspension.Methods:A reversed-phase high performance liquid chromatography(RP-HPLC)method was adopted.The Gemini C 18(4.6 mm×250 mm,5m)was used as separation column.And the mobile phase was a mixture of CH3OH-H2O(the volume ratio was 82:18,V/V),and the flow rate was 1.0 ml/min,and UV detection wavelength was 244 nm.And the temperature of column was 25℃.The influence of atomization temperature on the stability of inhaled Budesonide suspension was determined.Results:The retention time of Budesonide standard substance was 6 min,and the separating degree between Budesonide and other components was greater than 1.5.The relative standard deviation(RSD)of precision test was 0.46%,and the sample solution was stable within 24h.And there was a well linear relation between the concentration range of Budesonide(0.01~0.15 mg/mL)and peak area,and the linear equation was:A=5×107c+20336(r=0.9999).The average recovery of Budesonide among various batches was 96.35%(RSD=1.01%,n=3).The highest temperature at the center point of the bottom of medicine cup of ultrasonic atomizer did not exceed 46℃,and the sample solution was stable within 80℃.Conclusion:The RP-HPLC method has better precision and higher accuracy in determining inhaled Budesonide suspension.And Budesonide can remain stable during atomization and does not be affected by temperature changes in this method.