电感耦合等离子体质谱法测定索非布韦原料药锡的残留量

Assay Determination of Tin Residue in Sofosbuvir by ICP-MS

建立电感耦合等离子体质谱法测定索非布韦原料药锡的残留量,并进行方法学考察。将样品置于微波罐中,加入9 m L硝酸,150℃预消解5 min,再用微波消解仪快速消解,消解结束后将消解液置于150℃赶酸仪上赶酸至1 m L以下,将消解液转移至10 m L塑料量瓶中,用纯水定容至刻度,量取溶液,注入电感耦合等离子体质谱仪(ICP-MS)测定。结果表明,锡在0 ug/L^20 ug/L浓度范围内与离子强度呈良好的线性关系(r=0.999 8);精密称取本品7份,检出锡的含量,相对标准偏差(RSD)(n=7)为6.52%,重复性良好;锡对照品溶液重复进样6次,RSD(n=6)为4.05%,进样精密度良好;样品的加样回收率在97%~103%范围内,表明该测定方法的准确度良好。该方法简便、快速、重复性好、精密度好、准确度好。

To establish an ICP-MS method for assay determination of tin residue in Sofosbuvir. The methodological study was also conducted. The sample was placed in a microwave tank,9 m L of nitric acid was added,andthe digestion was carried out at 150°C for 5 minutes. The digestion solution was quickly digested with a micro-wave digestion. After digestion,the digestion solution was transferred to 1 m L or less at 150°C,10 m L plastic mea-suring bottle,constant volume with pure water. The solution was injected into the ICP-MS determination. The linear range of tin is 0 ug/L ~20 ug/L;reproducibility is good when the RSD of 7 batches samples is 6.52 %. The in-jection precision is good with RSD 4.05 %. The sample recovery rate is in the range of 97 % ~103%. The method is simple,and has good reproducibility,accuracy and precision,which is suitable for the assay determinationof tin residue in Sofosbuvir.