离子色谱法测定三磷酸腺苷二钠制剂中主成分及有关物质的含量  

Determination of principal components and related substances in adenosine disodium triphosphate preparation by ion chromatography

作　　者：山广志[1] 宗艳平 王晓 卢静华[2] 

机构地区：[1]中国医学科学院医药生物技术研究所,北京100050 [2]辽宁医学院药学院,辽宁锦州121000 [3]烟台东诚药业集团股份有限公司,山东烟台264006

出　　处：《色谱》2014年第11期1275-1279,共5页Chinese Journal of Chromatography

基　　金：科技部新药创制重大专项平台项目(2012ZX09301002-001-019)

摘　　要：建立了用于三磷酸腺苷二钠制剂中主成分及有关物质含量测定的离子色谱方法。采用 IonPac AS11-HC 色谱柱，以 KOH 溶液为淋洗液，梯度洗脱，流速为1.0mL / min，进样10μL，以 Dionex AERS 5004-mm 抑制器的电导检测器检测，三磷酸腺苷二钠（ATP-Na2）的含量按峰面积以外标法计算，二磷酸腺苷二钠（ ADP-Na2）及单磷酸腺苷二钠（AMP-Na2）按加校正因子的主成分自身对照法计算，未知杂质按主成分自身对照法计算。 ATP-Na2、ADP-Na2及 AMP-Na2的线性范围分别为0.000146-1.83 g / L、0.000484-1.51 g / L 及0.000426-0.804 g / L，相关系数分别为0.9997、0.9996及0.9999；对照品溶液在24 h 内的稳定性良好（峰面积 RSD 分别为1.3％、1.4％、2.5％）；ATP-Na2、ADP-Na2、AMP-Na2的方法定量限（S / N =10）分别为1.5 ng、4.8 ng、4.3 ng，检出限（S / N =3）分别为0.58 ng、1.21 ng、1.28 ng；ATP-Na2在3个水平的加样回收率分别为96.50％、96.57％和96.77％。本方法适用于三磷酸腺苷二钠制剂的质量控制。A new method was developed for the determination of adenosine disodium triphos-phate（ ATP-Na 2 ）and its related substances in ATP-Na 2 preparation by ion chromatography （IC）. The sample was diluted with ultrapure water and filtrated by 0. 22 μm polyether sulfone filter membrance,and then analyzed by IC directly without any more pretreatment. The analysis was performed on a Dionex IonPac AS11-HC column（250 mm×4 mm）and a guard column Ion-Pac AG11-HC（50 mm×4 mm）. A KOH eluent generator cartridge was used for gradient elution at the flow rate of 1. 0 mL / min. The detection was performed by a Dionex suppressed（Dionex AERS 500 4-mm）conductivity detector. The injection volume was 10 μL. The assay was quanti-tatively completed by external standard method and the related substances were calculated with correction factors. The linear ranges of the method for ATP-Na 2 ,adenosine disodium diphos-phate（ADP-Na2 ）and adenosine disodium monophosphate（ AMP-Na 2 ）were 0. 000 146 - 1. 83 g / L（r = 0. 999 7）,0. 000 484-1. 51 g / L（ r = 0. 999 6）and 0. 000 426- 0. 804 g / L（ r = 0. 999 9）, respectively. The average recoveries of ATP-Na 2 were 96. 50% ,96. 57% and 96. 77% at three spiked levels. The limits of quantitation（ S / N = 10）of ATP-Na 2 ,ADP-Na 2 and AMP-Na 2 were 1. 5 ng,4. 8 ng,4. 3 ng,and the limits of detection（S / N = 3）were 0. 58 ng,1. 21 ng,1. 28 ng, respectively. The results demonstrated that the system has the advantages of high sensitivity, facile automation and simple sample pretreatment. The method is suitable for the quality control of adenosine disodium triphosphate preparations.

关 键 词：离子色谱法 电导检测器 三磷酸腺苷二钠 有关物质 制剂 

分 类 号：O658[理学—分析化学]