生脉注射液中34种重金属元素测定方法研究OA

In accordance with the relevant guidelines of ICH Q3D(R2)Guideline for Elemental Impurities,an analytical method was established for the simultaneous determination of 34 heavy metal elements in Shengmai injection by ICP-MS.The test solution was ablated under microwave,then diluted and analyzed by ICP-MS method.The assay data were further calibrated by adding In and Sc as the internal standard.The plasma output power was set at 1 150 W,the sampling depth was 8 mm,the maximum carrier gas volume was 1.045 L/min,the cooling gas was 14 L/min and the auxiliary gas was 0.9 L/min.The peristaltic pump speed was 40 r/min,the feeding system was acid-resistant system,with nickel material for the sampling and interception cones.The sampling method was manual,and the assay was repeated 3 times.As a result,our method demonstrated excellent linearity for the 34 heavy metal elements(r＞0.99),with the average recoveries ranging from 70%to 120%.In addition,both reproducibility RSD and the intermediate precision RSD were less than 25%.Our analysis of 6 batches of Shengmai injectionsshowed the 34 heavy metal elements met the requirements of ICH Q3D.Overall,we developed a convenient,rapid,sensitive and accurate method for the determination of the concentrations of 34 heavy metal elements in Shengmai Injections.Based on our preliminary methodological validation,the safety of Shengmai Injection can bebroadly monitored,and ourmethod can provide a basis for more rigorous quality management in this area.