离子色谱法测定化学对照品中5种酸根的含量  

Determination of five acid radicals in chemical reference substances by ion chromatography

作　　者：马玲云[1] 孟雨馨 翟晨斐 冯玉飞[1] 刘倩[1] 牛剑钊[1] 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)

机构地区：[1]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2024年第10期1741-1748,共8页Chinese Journal of Pharmaceutical Analysis

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.

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 

分 类 号：R917[医药卫生—药物分析学]