间接紫外检测离子色谱法测定托吡酯片的无机降解产物

目的 建立测定托吡酯片中无机降解产物硫酸盐和氨基磺酸盐的间接紫外检测离子色谱法.方法 采用Hamilton PRP-X100阴离子交换色谱柱(250mm×4.6mm,5μm),流动相为4.5mmol/L对羟基苯甲酸溶液(用15%氢氧化钠溶液调节pH至9.9±0.1)-甲醇(97.5:2.5),检测波长为310 nm,检测器极性为负,流速2.0 mL/min,进样量100μL,柱温为40℃.结果 硫酸盐(以SO42-计)的线性质量浓度范围为24.673～98.692μg/mL,r=0.999 98(n=5);平均加样回收率为98.44%,RSD=1.65%(n=9).氨基磺酸盐(以NH2SO3-计)的线性质量浓度范围为30.063～120.252μg/mL,r=0.999 95(n=5);平均加样回收率为99.83%,RSD=0.96%(n=9).结论 所建立的方法灵敏度高、专属性强、重现性好,可用于测定托吡酯片中无机降解产物硫酸盐和氨基磺酸盐的含量.

Determination of Inorganic Degradation Products in Topiramate Tablets by Ion Chromato- graphic Method with Indirect UV Detection

Objective To develop an ion chromatographic method with indirect UV detection for the determination of sulfate and sulfamate as inorganic degradation products in topiramate tablets. Methods The samples were analyzed on the Hamilton PRP-X100 anion exchange column （250 mm×4. 6 mm,5 um）.The mobile phase was 4.5 mmol/L 4-hydroxy benzoic： acid solution （adjusting pH to 9.9 ± 0.1 with 15% NaOH solution） - methanol （97.5 ： 2. 5）. The UV - detector was set at 310 nm with negative polarity. The flow was 2. 0 mL/min. The injection volume was 100 uL and the column temperature was 40 ℃. Results The linear range of sulfate （calculated on SO4 2-） was 24. 673-98. 692 ug/mL, r=0. 999 98 （n =5）. The average recovery rate was 98.44%, RSD = 1.65% （ n = 9）. The linear range of sulfamate （calculated on NH2SO3 ） was 30. 063 - 120. 252 ug/mL, r = 0. 999 95 （ n = 5）. The average recovery rate was 99. 83%, RSD =0. 96% （n =9）. Conclusion The established method is sensitive, specific, repeatable and suitable for the determination of sulfate and sulfamate as the inorganic degradation products in topiramate tablets.