2种方法测定咪唑斯汀缓释片含量

目的: 建立咪唑斯汀缓释片的高效液相色谱测定方法和紫外分光光度测定方法,比较2种方法之间的优缺点。 方法: 高效液相色谱法采用Apollo C₁₈(250 mm×4.6 mm,5 μm)柱分离,流动相:0.05 mol·L^-1磷酸二氢钾(以0.1 mol·L^-1氢氧化钾调节pH至6.8)-甲醇-乙腈(45∶ 10∶ 45),流速0.8 mL·min^-1,检测波长216 nm,柱温30 ℃。紫外分光光度法溶剂为0.005 mol·L^-1的盐酸溶液,含量测定浓度为10 μg·mL^-1的溶液;测定波长为287 nm。 结果: 高效液相色谱法咪唑斯汀在0.1.0 ng~2.5×10³ ng范围内线性关系良好(A=8916.2C+10.015,r=1.0000);高、中、低3种浓度的加样回收率(n=3)分别为99.8%(RSD=0.13%),100.0%(RSD=0.27%),100.0%(RSD=0.35%);日内精密度RSD=0.10%(n=6)。紫外分光光度法咪唑斯汀的浓度在2.00~20.00 μg·L^-1范围内线性关系良好(A=468×10^-4C+7×10^-4,r=0.9999);高、中、低3种浓度的加样回收率(n=3)分别为100.4%(RSD=0.21%),100.6%(RSD=0.43%),100.4%(RSD=0.57%);日内精密度RSD=0.12%(n=6)。 结论: 尽管紫外分光光度法测量操作简单快速,可是高效液相色谱法有更高的专属性且灵敏度高,适用于咪唑斯汀缓释片的含量及有关物质的测定。

Objective: To establish the HPLC and UV methods for determination of mizolastine and compare with the different between two methods. Methods: HPLC with a column of Apollo C₁₈(250 mm×4.6 mm,5 μm),the 0.05 mol·L^-1 potassium dihydrogen phosphate(adjust pH to 6.8 with 0.1 mol·L^-1 potassium hydroxide)-methanol-acetonitrile(45∶ 10∶ 45)as mobile phase,the flow rate was 0.8 mL·min^-1,the detection wavelengths were 216 nm,the column temperature was 30 ℃.UV solvent was 0.005 mol·L^-1 hydrochloric acid solution.The determination concentration of content 10 μg·mL^-1. Results: HPLC calibration curve was linear within the range of 0.1-2.5×10³ ng(A=8916.2C+10.015,r=1.0000).The mean recoveries (n=3) of high,middle and low concentrations were 99.8%(RSD=0.13%),100.0%(RSD=0.27%),100.0%(RSD=0.35%)respectively.Intre-day RSD=0.10%(n=6).UV calibration cure had good linearity in the range of 2.00-20.00 μg·L^-1(A=468×10^-4C+7×10^-4,r=0.9999),the mean recoveries (n=3) of high,middle and low concentrations were 100.4%(RSD=0.21%),100.6%(RSD=0.43%),100.4%(RSD=0.57%)respectively.Intre-day RSD=0.12%(n=6). Conclusion: Although the UV method is simple and rapid,but the established HPLC method is sensitive and accurate for determination of Mizolastine content and even relative substances contained.