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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ApolloC18(250mm×4.6mm,5μm)柱分离,流动相:0.05mol·L-1磷酸二氢钾(以0.1mol·L-1氢氧化钾调节pH至6.8)-甲醇-乙腈(45∶10∶45),流速0.8mL·min-1,检测波长216nm,柱温30℃。紫外分光光度法溶剂为0.005mol.L-1的盐酸溶液,含量测定浓度为10μg.mL-1的溶液;测定波长为287nm。结果:高效液相色谱法咪唑斯汀在0.1.0ng～2.5×103ng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2.00～20.00μg.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 a method for the determination of mizolastine sustained-release tablets by high performance liquid chromatography and ultraviolet spectrophotometry, and to compare the advantages and disadvantages between the two methods. METHODS: High performance liquid chromatography (HPLC) was performed on a Apollo C18 column (250 mm × 4.6 mm, 5 μm). The mobile phase consisted of 0.05 mol·L -1 potassium dihydrogen phosphate (adjusted to pH 6.8 with 0.1 mol·L -1 potassium hydroxide) Methanol-acetonitrile (45:10:45), flow rate 0.8mL · min-1, detection wavelength 216nm, column temperature 30 ℃. UV spectrophotometry solvent 0.005mol.L-1 hydrochloric acid solution, the concentration of the determination of the solution was 10μg.mL-1; determination wavelength of 287nm. Results: Mizolastine in the range of 0.1.0ng ~ 2.5 × 103ng had a good linearity (A = 8916.2C + 10.015, r = 1.0000). The recoveries of high, medium and low concentrations n = 3) were 99.8% (RSD = 0.13%), 100.0% (RSD = 0.27%) and 100.0% (RSD = 0.35%) respectively. Intraday precision RSD was 0.10% (n = 6). The concentration of mizolastine in UV spectrophotometry was good in the range of 2.00 ~ 20.00μg.L-1 (A = 468 × 10-4C + 7 × 10-4, r = 0.9999); high, medium and low The average recoveries (n = 3) were 100.4% (RSD = 0.21%), 100.6% (RSD = 0.43%) and 100.4% (RSD = 0.57% 6). Conclusion: Although UV spectrophotometry is simple and fast, HPLC is more specific and sensitive and suitable for the determination of mizolastine sustained-release tablets and related substances.