212165寡核苷酸类抗流感药物钠含量测定仲婕.docVIP

寡核苷酸抗流感药物钠含量测定 仲婕1,2，李保山1,2，朱德领1,2*，张金钟1,2，施明珠1,2 杭州天龙药业有限公司，浙江杭州 310021； 2.军科天龙药物研究院，浙江杭州 310021） 摘要：目的：用、原子吸收光谱1mL·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97.2%和89.5%，线性方程分别为：Y=105.22X=0.1007,r=1.0000,Y=0.2894X+0.006, r=0.9991；测量结果无显著性差异，配对t检验P＞0.05；Bland -Altman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：离子色谱法的重现性和回收率均优于原子吸收法；Bland -Altman法综合判断两组数据具有高度的一致性。 关键词：离子色谱法;原子吸收光谱Study on the content of sodium in oligonucleotide bulk pharmaceuticals ZHONG Jie1,2，LI Bao-shan1,2 ZHU De-ling1,2* ZHANG Jing-zhong1,2，，SHI Min-zhu1,2 (1.Hangzhoutianlong Pharmaceutinal CO.,Ltd.，Hangzhou 310021, China; 2. Institute of Junketianlong Materia Medica, Hangzhou 310021, China ) ABSTRACT: OBJECTIVE Determination of sodium content in oligonucleotide bulk pharmaceuticals by ion-chromatography and atomic absorption spectrophotometry. To evaluate the the degree of agreement between measurements. METHODS The precision,linearity, repeatability and analytical recovery were evaluated on Dionex ICS900 and Shimadzu AA-6300C. By using paired t test and Bland-Sltman method to estimate consistency of two kinds of instrument and decide whether the data is replaceability or not. 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 97.2%(RSD=2.46%,n=6) and 89.5%(RSD=8.59%,n=6) for ion-chromatography and atomic absorption spectrophotometry,respectively. The mean difference was -0.0136% with 95% confidence interval -1.514 to 1.487.Most of the differences lay between these limist (between d-1.96s and d+1.96S). CONCLUSION There is no significant difference compared with the standard method—flame absorption spectrum method. Moreover, the ion-chromatography method had demonstrated its superiority in repeatability and analytical recovery. KEY WORDS: IC;AAS;comparison;paired t test; bland-altman method; the degree of agreement 钠离子的电