离子色谱法测定药物那曲肝素钙中游离硫酸根含量  

IC Determination of Free Sulfate Ion in the Drug Nadroparinum Calcium

作　　者：胡平[1] 杨力学[1] 

机构地区：[1]石家庄市疾病预防控制中心,石家庄050011

出　　处：《理化检验（化学分册）》2011年第1期90-91,共2页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：将药物试样溶解于水中,定容为100 mL后经0.22μm滤膜过滤,离子色谱法测定滤液中游离硫酸根含量。采用AS11-HC型阴离子色谱柱进行分离,用22 mmol·L^-1氢氧化钾溶液等度淋洗,流量1.0 mL·min^-1,抑制电流55 mA。在此检测条件下,游离硫酸根质量浓度在0.50-10.0 mg·L^-1范围内与对应的峰面积呈线性关系,方法的检出限（3s/k）为0.003μg·g^-1。在3个浓度水平上进行精密度试验,测得相对标准偏差（n=7）均小于2%。以3个药物试样作基体加入标准溶液作回收试验,测得平均回收率在102.0%-106.0%之间。The drug sample was dissolved in water and diluted to 100 mL in a volumetric flask.The solution was filtered with filtering membrane of 0.22 μm and the filtrate was used for IC determination of free sulfate ion.The Dionex AS11-HC column was used for separation with 22 mmol·L^-1 KOH solution as mobile phase with a flow-rate of 1.0 mL·min^-1.Conductivity detector with depression current of 55 mA was used in the determination.Linear relationship between values of peak area and mass concentration of SO2-4 ion was obtained in the range from 0.50 to 10.0 mg·L-1,and detection limit（3s/k） found was 0.003 μg·g^-1.Precision was tested at 3 concentration levels and values of RSD′s（n=7） found were less than 2%.Test for recovery was made by standard addition method using 3 drug samples as matrixes.Values of average recovery found were from 102.0% to 106.0%.

关 键 词：离子色谱法 那曲肝素钙 游离硫酸根 

分 类 号：O652.63[理学—分析化学]