离子色谱法测定复方聚乙二醇电解质散(Ⅲ)中氯离子、硫酸根和碳酸氢根的含量

Determination of chloride,sulfate and bicarbonate ions in Polyethylene glycol electrolyte powder(Ⅲ)by ion chromatography

目的建立同时测定复方聚乙二醇电解质散(Ⅲ)中氯离子、硫酸根和碳酸氢根含量的离子色谱法。方法色谱柱为Dionex Ionpac^(TM) AS11-HC阴离子分析柱,保护柱为Dionex IonPac^(TM) AG11-HC,以10 mmol/L氢氧化钾为淋洗液进行等度洗脱,流速为1.2 mL/min,检测器为电导检测器,抑制器为Dionex AERS,抑制电流为30 mA,柱温为30℃,进样体积为10μL;按外标法计算氯离子和硫酸根的含量,按双对数拟合的标准曲线法计算碳酸氢根的含量。结果该色谱条件下,氯离子、硫酸根、碳酸氢根能有效分离,其线性范围分别为0.055~0.219 mg/mL(r为0.9999)、0.155~0.618 mg/mL(r为1.0000)、0.065~0.121 mg/mL(r为0.9999);回收率分别为98.06%~101.34%、97.37%~101.25%、97.16%~99.81%,RSD分别为1.1%、1.3%、1.0%(n=9);精密度、准确度、稳定性、耐用性考察的RSD均小于2%。结论建立的离子色谱法简单快速,准确度、精密度和耐用性良好,可同时测定复方聚乙二醇电解质散(Ⅲ)中氯离子、硫酸根、碳酸氢根的含量,适用于该药品的质量控制。

OBJECTIVE To establish an ion chromatography method for the simultaneous determination of chloride,sulfate and bicarbonate ions in Polyethylene glycol electrolyte powder(Ⅲ).METHODS The chromatographic column was a Dionex Ionpac^(TM) AS11-HC anion analysis column,with a Dionex IonPac^(TM) AG11-HC guard column.The mobile phase was 10 mmol/L potassium hydroxide at an isocratic elution flow rate of 1.2 mL/min.The detector was a conductivity detector,and the suppressor was a Dionex AERS with a suppressor current of 30 mA.The column temperature was maintained at 30℃,and the injection volume was 10μL.Chloride and sulfate contents were calculated by external standard method,while bicarbonate content was determined by double logarithmic fitting standard curve method.RESULTS Under these chromatographic conditions,chloride,sulfate and bicarbonate ions were effectively separated with linear ranges of 0.055 to 0.219 mg/mL(r=0.9999),0.155 to 0.618 mg/mL(r=1.0000),and 0.065 to 0.121 mg/mL(r=0.9999),respectively.The recoveries were 98.06%to 101.34%,97.37%to 101.25%,and 97.16%to 99.81%,respectively,with RSDs of 1.1%,1.3%and 1.0%(n=9).The RSDs for the evaluation of precision,accuracy,stability and ruggedness were all less than 2%.CONCLUSIONS The established ion chromatography is simple,rapid,accurate,precise and durable,can simultaneously determine the contents of chloride,sulfate and bicarbonate ions in Polyethylene glycol electrolyte powder(Ⅲ),which is suitable for its quality control.