液相色谱法测定脑膜炎球菌结合物原液中残余二甲亚砜

Determination of the residual content of DMSO in meningococcal conjugates bulk of A,C,Y and W135 by HPLC

目的建立并验证脑膜炎球菌结合物原液中残余二甲亚砜的检测方法。方法采用液相色谱法,使用Kro-masil C18柱(250 mm×4.6 mm),25%甲醇溶液为流动相,二极管阵列检测器测定脑膜炎球菌结合物原液中残余二甲亚砜。结果二甲亚砜在1～100 mg/L的范围内相关系数r大于0.999,线性关系良好,平均回收率为94%～114%、变异系数为0.46%～0.89%,最小定量限为1.0 mg/L,远低于药典规定。结论该方法简便易行,结果准确。

Objective To establish a method for determination of the residual dimethylsulfoxide（DMSO） in meningococcal conjugates bulk of A,C,Y and W135.Methods HPLC was used in this test.The content of DMSO was analyzed with Kromasil C18 column（250 mm×4.6 mm）,the mobile phase was 25% methanol,and diode array detector was used as detector.Results A good liner correlation was obtained over the range of 1-100 mg / L,r 0.999.The average recovery of DMSO was 94%-114% and the average CV was 0.46%-0.89%.The method can quantify the DMSO with a minimum amount of 1.0 mg / L for the sensitivity at least 10 times higher than that of noise assay.This concentration was much lower than the limit concentration in pharmacopeia.Conclusions This method was easily operative and accurate for precise determination.