【摘要】 目的:建立定量测定含枸橼酸盐和蔗糖的血液制品或干热法病毒灭活中间制品中枸橼酸离子含量的高效液相分析方法,并与中国药典2005年版三部枸橼酸离子测定第二法进行比较。方法:采用RP-C18色谱柱以磷酸盐缓冲液作为流动相,以5 mmol·L-1枸橼酸离子溶液做回收率和精密度分析。选择5种共20个批次仅含枸橼酸盐不含有蔗糖的血液制品,按2005年版中国药典枸橼酸离子测定第二法平行分析,比较两者一致性。结果:RP-HPLC法枸橼酸离子保留时间大约在5min,其5次进样保留时间RSD%(n=5)为0.0,峰面积RSD%(n=5)为0.1,实验所测枸橼酸离子标准回收率大于99.0%,标准曲线线性相关系数r大于0.999。RP-HPLC法与IEC-HPLC法平行检测20个批次制品的枸橼酸离子含量,统计学结果显示2种方法相关系数r为0.9994,两者无显著差异(P>0.05)。结论:RP-HPLC法的准确性和精密度良好,与2005年版中国药典三部第二法结果一致并可规避其缺点,适用于含枸橼酸盐和蔗糖的血液制品及干热病毒灭活中间制品的枸橼酸离子含量分析,也可用于检测常规血液制品,可以作为2005年版中国药典枸橼酸离子测定的补充方法。更多还原

【Abstract】 Objective:To establish the quantitative determination method of sodium citrate by HPLC in citrate and sucrose containing blood products or dry-heat treated intermediate products.Comparison was also carried out between the developed method and ion exchange HPLC method published in ChP 2005.Methods:An HPLC method was developed to specifically determine sodium citrate on reversed-phase chromatography column with UV detection at 210 nm.The separations were performed at 40℃ on a Waters Symmetry sheild RP-C18 column with a mobile phase of phosphoric acid solution as elution.In each experiment 5 mmol·L-1 sodium citrate standard solution was detected with external standard method to mensurate recovery rate.Five kinds of blood products with a total of 20 batches derived from different manufactures were selected for sodium citrate determination.These products only contain sodium citrate but do not contain sucrose which makes it possible to use IEC-HPLC method issued in ChP 2005 and make it easier to do methodology comparison with RP-HPLC method.Samples were divided into two parts after pre-treatment to do comparison in the recovery rate,linear and consistency.Results:The results showed that the retention time of sodium citrate was in about 5 minutes.Sodium citrate standard solution was injected for 5 times to get recovery results which indicate that RSD(n=5)was 0.0%(calculated by retention time) and 0.1%(calculated by peak area),respectively.The average recovery was over 99.0% and linear correlation r was over 0.999.Statistical data showed that the amount of sodium citrate in 20 batches of blood products determined by RP-HPLC method and IEC-HPLC method has no significant difference(P>0.05) and the correlation coefficient r was 0.9994.These results demonstrated that RP-HPLC method and IEC-HPLC method are highly consistent in sodium citrate quantitative determination.Conclusion:The proposed RP-HPLC method is simple,accurate and.It can effectively avoid the shortcomings issued in ChP 2005 which can not detect total citrate in citrate and sugar containing blood products.The determination results of sodium citrate in blood products by RP-HPLC method were in good accordance with those from the IEC-HPLC method.High attention should be given to the developed RP-HPLC method and it can be widely applied as an effectively complemental way for sodium citrate determination for ChP 2005.更多还原