离子色谱法测定丁二磺酸腺苷蛋氨酸中的丁二磺酸

Determination of 1,4-butanedisulfonate anion in ademetionine 1,4-butanedisulfonate by Ion chromatography

目的采用离子色谱法测定丁二磺酸腺苷蛋氨酸原料药中丁二磺酸的含量。方法采用Dionex ICS 5000离子色谱仪,用IonpacAS14（250 mm×4 mm）阴离子交换色谱柱（分析柱）,流动相为3.5 mmoL·L^-1无水碳酸钠溶液-1.0 mmoL·L^-1碳酸氢钠溶液,流速2.0 mL·min^-1,电导检测器,进样量25μL。结果丁二磺酸0.037～558μg·mL^-1与峰面积的线性关系良好（r=0.9996）,平均回收率为99.9%,RSD=0.61%（n=9）,检出限为0.3 ng。结论所用方法可准确测定丁二磺酸腺苷蛋氨酸中丁二磺酸的含量,可有效控制其质量。

OBJECTIVE To establish an ion chromatography method for determination of 1,4 - butanedisulfonate anion of ademe- tionine 1,4 - butanedisulfonate. METHODS Dionex ICS 5000 ion chromatography was used. The Ionpac AS14 anion analytical column（250 mm× 4 mm） was used with the mixture of 3.5 mmoL· L^-1 sodium carbonate and 1.0 retooL· L^-1 sodium hydrogen carbonate as the mobile phase. Conductivity detector was employed, and the flow rate was 2.0 mL· min^-1, while the injection volume was 25 μL. RESULTS A good linearity for the content of 1,4 - butanedisulfonate was found in the range of 0. 037 - 558 μg·mL ^- 1 （ r = 0. 9996）. The average recovery was 99.9% （ RSD = 0.61%, n = 9）, and the minimum detection limit was 0.3 ng. CONCLUSION The method could accurately detect 1,4 -butanedisulfonate in ademetionine 1,4 -butanedisulfonate, and can be used as an effective methed for the quality control of ademetionine 1,4 - butanedisulfonate.