摘要
目的:建立适用于同时测定含甲磺酸、盐酸、磷酸、硫酸、丁二磺酸化学对照品中酸根含量的离子色谱法。方法:采用Metrosep A Supp 5250/4.0(250 mm×4.0 mm,5μm)色谱柱,以6.4 mmol·L^(-1)碳酸钠溶液-2.0 mmol·L^(-1)碳酸氢钠溶液为淋洗液,等度洗脱,流速0.7 mL·min^(-1),柱温30℃。结果:甲磺酸根(19.1~71.7μg·mL^(-1))、氯离子(2.6~25.8μg·mL^(-1))、磷酸根(7.0~26.3μg·mL^(-1))、硫酸根(6.8~51.0μg·mL^(-1))和丁二磺酸根(21.3~105.5μg·mL^(-1))在各自范围内线性关系良好(r≥0.9995);精密度(RSD≤2%)、稳定性(RSD≤2%)、重复性(RSD≤2%)良好;平均加样回收率(n=9)为98%~102%,以成盐形式计算,甲磺酸氨氯地平中甲磺酸含量为23.69%,盐酸胍法辛中盐酸含量为12.66%,磷酸瑞格列汀中磷酸含量为17.38%,硫酸沙丁胺醇中硫酸含量为16.49%,丁二磺酸腺苷蛋氨酸中丁二磺酸含量为45.61%,理论值与测定值偏差均<0.50%。结论:该方法适用性良好,可用于含甲磺酸、盐酸、磷酸、硫酸、丁二磺酸化学对照品中酸根的筛查及含量测定。
Objective:To establish an ion chromatography method suitable for simultaneous determination of acid radical content in chemical reference substances containing methanesulfonic acid,hydrochloric acid,phosphoric acid,sulfuric acid and butadisulfonic acid.Methods:The chromatographic column of Metrosep A Supp 5250/4.0(250 mm×4.0 mm,5μm)was used with 6.4 mmol·L^(-1)Na_(2)CO_(3)and 2.0 mmol·L^(-1)NaHCO_(3)as the eluent with a flow rate of 0.7 mL·min^(-1).Column temperature was 30℃.Results:Methanesulfonate(19.1-71.7μg·mL^(-1)),chloride ion(2.6-25.8μg·mL^(-1)),phosphate(7.0-26.3μg·mL^(-1)),sulfate(6.8-51.0μg·mL^(-1)),and succinate(21.3-105.5μg·mL^(-1))had good linear relationships within their respective ranges(r≥0.9995).Precision(RSD≤2%),stability(RSD≤2%)and repeatability(RSD≤2%)were good.The average recovery rates(n=9)were 98%-102%.Calculated as salt formation,the content of mesylate in amlodipine mesylate was 23.69%,the content of hydrochloric acid in guanfacine hydrochloride was 12.66%,the content of phosphoric acid in reagliptin phosphate was 17.38%,the content of sulphate in salbutamol sulfate was 16.49%,and the content of butyldisulfonic acid in adenosine butyldisulfonic acid was 45.61%.The deviation between theoretical and measured values was less than 0.50%.The measured values were close to the theoretical values.Conclusion:The method is suitable for the screen and determination of acid radicals in chemical reference products containing methanesulfonic acid,hydrochloric acid,phosphoric acid,sulfuric acid and butadisulfonic acid.
作者
马玲云
孟雨馨
翟晨斐
冯玉飞
刘倩
牛剑钊
MA Ling-yun;MENG Yu-xin;ZHAI Chen-fei;FENG Yu-fei;LIU Qian;NIU Jian-zhao(National Institutes for Food and Drug Control,Beijing 100050,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2024年第10期1741-1748,共8页
Chinese Journal of Pharmaceutical Analysis
关键词
甲磺酸
盐酸
磷酸
硫酸
丁二磺酸
含量测定
化学对照品
离子色谱法
methanesulfonic acid
hydrochloric acid
phosphoric acid
sulfuric acid
butadisulfonic acid
content determination
chemical reference substance
ion chromatography
