HPLC法测定甲苯磺丁脲片溶出度的研究

Determination of Dissolution Method of Tolbutamide Tablets by HPLC

目的建立高效液相色谱(HPLC)法测定甲苯磺丁脲片的溶出度。方法根据甲苯磺丁脲片的溶解性和吸收特性,采用浆法测定溶出度,以磷酸盐缓冲液(pH 6.8)900 mL为溶出介质,转速为75 r/min,取样时间为30 min。液相色谱条件:用十八烷基硅烷键合硅胶为填充剂色谱柱(250 mm×4.6 mm,5μm);流动相为磷酸二氢钾溶液(取磷酸二氢钾1.36 g,加水1000 mL使溶解,用磷酸调节pH值至3.5)-乙腈(65∶35);检测波长230 nm;流速1.0 mL/min;柱温:35℃;进样体积20μL。结果甲苯磺丁脲在0.005023~0.5023 mg/mL范围内呈现良好的线性关系(r=1.0000,n=5);平均回收率为100.0%,RSD为0.8%(n=9)。结论拟定的溶出试验测定方法准确可靠、干扰少,可用于甲苯磺丁脲片的溶出度检查。

Objective To establish a HPLC method for determination the dissolution of tolbutamide tablets.Methods According to the dissolution and absorption characteristics of tolbutamide tablets,adopted the second method(paddle method)for dissolution.The dissolution medium was 900 mL of phosphate buffer solution(pH 6.8),and rotate speed was 75 r/min.The sampling time was 30 min,and the liquid chromatographic condition of column was octadecylsilane bonded silica gel column(250 mm×4.6 mm,5μm),the mobile phase was potassium dihydrogen phosphate solution(1.36 g of potassium dihydrogen phosphate was taken,1000 mL of water was added to dissolve,and the pH value was adjusted to 3.5 with phosphoric acid)-acetonitrile(65∶35),the wavelength of UV detector was 230 nm;the flow rate was 1.0 mL/min;the column temperature was 35℃;the injection volume was 20μL.Results The calibration curve was liner in the concentration range of 0.005023~0.5023 mg/mL,r=1.0000(n=5).The average recoveries was 100.0%with RSD of 0.8%(n=9).Conclusion The established method is accurate,reliable and minimal interference to determine the dissolution of tolbutamide tablets.