寡核苷酸抗流感药物流感泰得钠含量测定

Study on the Content of Sodium in Oligonucleotide Bulk Pharmaceuticals-Flutide

关键词:  离子色谱法  原子吸收光谱法  钠含量  t检验  Bland-Altman法  一致性

Key words:  IC  AAS  sodium content  paired t test  bland-altman method  the degree of agreement

摘要:

目的 用离子色谱法(IC)、原子吸收光谱法(AAS)评价抗流感药物钠含量，探讨两种测量方法定量结果的一致性。方法 在戴安ICS900离子色谱仪上，用阳离子分析柱Ionpac CS12(4 mm×250 mm)，流动相：甲烷磺酸；抑制型电导检测；流速1 mL·min^-1；测量结果与国标方法(火焰原子收光谱法)进行方法学评价比较；应用配对t检验和Bland -Altman法对两种测量方法进行一致性评价。结果 两种方法的精密度分别为2.0%和0.7%，重现性分别为2.0%和7.96%，回收率分别为99.6%和89.8%，测量结果无显著性差异，配对t检验P>0.05；Bland-Altman法一致性评价的95%一致性界限为：(-1.514，1.487)，绝大多数差值都位于该区间内。结论 IC的重复性和回收率均优于AAS；Bland-Altman法综合判断两组数据具有高度的一致性。

Abstract:

OBJECTIVE To determine sodium content in oligonucleotide bulk pharmaceuticals by ion-chromatography and atomic absorption spectrophotometry. To evaluate the degree of agreement between measurements. METHODS Ion chromatography (IC) was carried out by using an Ion-pac CS12 column (4 mm×250 mm) with methanesulfonic acid as the mobile phase, suppressed conductivity detector, on Dionex ICS 900. The results was compared with atomic absorption spectrophotometry (AAS) method provided by national standard. By using paired t test and Bland-Sltman method to estimate consistency of two methods. RESULTS The two method results showed that the precision were 2.0% and 0.7%, the repeatability were 2.0% and 7.96%, the analytical recovery were 99.6% and 89.8% for ion-chromatography and atomic absorption spectrophotometry, respectively. The mean difference was -0.0136% with 95% confidence. CONCLUSION There is no significant difference compared with the national standard method-AAS. Moreover, the ion-chromatography method had demonstrated its superiority in repeatability and analytical recovery.