注射用亚锡亚甲基二膦酸盐含量测定方法改进

Improvement on assay method of Methylene diphosphonate and Stannous Chloride for Injection

目的:建立电感耦合等离子体发射光谱(ICP-OES)方法,测定注射用亚锡亚甲基二膦酸盐中磷、锡元素的含量,为简化本品含量测定方法提供参考。方法:采用ICP-OES方法,仪器参数:发射功率(RF)1150 W,泵速75 r·min-1,辅助气体流量0.5,雾化气体流量0.7,驱气气体流量一般,在此条件下进行磷和锡元素的含量测定方法并对上市产品进行了检测。结果:两种待测元素专属性良好,稳定性良好,线性良好,r=0.9995,相对标准偏差在0.02%~0.47%,磷元素平均回收率为99.9%,RSD为0.66%,锡元素平均回收率为99.8%,RSD为1.39%。磷元素检出限为0.0114 mg·L-1,定量限为0.038 mg·L-1,锡元素检出限为0.0441 mg·L-1,定量限为0.147 mg·L-1。经对上市品进行测定,磷的含量范围在98.9%~99.5%之间,锡的含量范围在100.2%~102.9%之间,测定结果重现性好。结论:该方法速度快、耗时短、线性范围宽、选择性好、干扰少、检出限低,是一种准确、快速、有效的方法。

Objective:To establish an ICP-OES method for the determination of phosphorus and tin in Methylene diphoshonate and Stanous Chloride for Injection.Method:The ICP-OES method was used.The instrument parameters were as follow:emission power(RF)1150 w,pump speed 75 r·min-1,auxiliary gas flow 0.5,atomization gas flow 0.7,and purge gas flow in general.Results:There were good specificity,stability and linearity for determination of two elements of phosphorus and tin.The coefficient was 0.9995,and the relative standard deviations were 0.02%to 0.47%.The average recovery of phosphorus was 99.9%with RSD as 0.66%,and the average recovery of tin was 99.8%with RSD as 1.39%.The limit of detection of phosphorus was 0.0114 mg·L-1,and the limit of quantitation was 0.038 mg·L-1.The limit of detection of tin was 0.0441 mg·L-1,and the limit of quantitation was 0.147 mg·L-1.The test results showed that the contents of phosphorus fell into 98.9%-99.5%,and the contents of tin fell into 100.2%-102.9%.The test results had the good reproducibility.Conclusion:The established method has the advantages of fast test,less time consuming,wide linear range,good selectivity,less interference and low limit of detection.It is an accurate,rapid and effective method.