口服补液盐ii中总钠和钾含量的测定 - 中国药品标准杂志.doc

原子吸收分光光度（广州市药品检验所，广州 510160） 吸收分光光度法方法通过考察消电离剂氯化锶的作用及加入量，用原子吸收分光光度法测定聚丙烯酸钠含量。结果钠在0～0.6 mg·L-1范围内浓度与吸光度相关系数为0.99 (n = 6)，特征浓度为0.01mg·L-1，回收率在97.2％～102.4％之间，RSD为1. %（n = 9）。结论修订方法聚丙烯酸钠的含量。 关键词：原子吸收分光光度法；聚丙烯酸钠；锶 Improvement Discussion on Determination of the Sodium Polyacrylate Content by Atomic Absorption Spectrophotometry Li Chunying, He Yufen (Guangzhou Institute for Drug Control, Guangzhou 510160 ) Abstract Objective: To improve and discuss the atomic absorption spectrophotometry (AAS) method to determine the content of Sodium Polyacrylate. Methods: The strontium chloride solutions were added into the sample solutions to eliminate the ionization interference, and the linear calibration range of the reference solutions was adjusted. Then the improved AAS method was used to determine the content of sodium polyacrylate. The calculated contents were compared to that obtained by inductively coupled plasma-mass spectrometry (ICP-MS) method. Results: The linear calibration range was 0 to 0.6 mg·L-1, and the correlation coefficient between concentration and absorbance was 0.9990 (n = 6). The characteristic concentration was 0.011 mg·L-1. The recovery was between 97.2% and 102.4% with RSD as 1.8 % ( n=9). There was no difference between the results obtained by the improved AAS and ICP-MS methods. Conclusion: This improved method is accurate, convenient, and suitable for determination of the Sodium Polyacrylate content. Key words: atomic absorption spectrophotometry; Sodium Polyacrylate; strontium 聚丙烯酸钠为丙烯酸中和或部分中和聚合的产物，作为药用辅料，被用作合剂、增稠剂及乳化分散剂。聚丙烯酸钠在各国药典中均未收载，目前该品种仅有食品添加剂的国家标准（GB29948-2013）及进口药品注册标准（J前者未收载含量测定项目，后者采用原子吸收法AAS）测定聚丙烯酸钠的含量。在2015年版《中国药典》增修订聚丙烯酸钠标准含量测定方法存在以下问题：标准曲线范围为1.5～5 mg·L-1（以钠计），其吸光度值均超过1，若通过调整仪器参数降低灵敏度，其重现性变差且操作繁琐，[1]、口服补液盐散（III）[2]及相关文献[]均采用火焰原子吸收法测钠标最高点一般1 mg·L-1；②加样回收试验测得回收率达182%样品采用炽灼残渣的方法进行前处理，若使用瓷坩埚或石英坩埚易出现粘连及炽灼不完全的情况。针对上述电感耦合等离子体质谱法进行，修订方法聚丙烯酸钠的含量。 1仪器与试药 iCE3500型原子吸收分光光谱仪热电公司； 7900型电感耦合等离子体质谱仪安捷伦公司；钠空心阴极灯（北京曙光明电子光源仪器有限公司，最大工作电流为0 mA）