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目的:建立离子色谱法同时测定硬脂酸镁中的氯离子和硫酸根离子的含量,并评价不同级别硬脂酸镁中氯离子和硫酸根离子含量的质量状况。方法:采用Dionex Ion Pac AS18(4 mm×250 mm)色谱柱,10、40 mmol·L~(-1)氢氧化钾淋洗液,梯度洗脱,流速为1.0 m L·min~(-1),进样量为25μL,标准曲线法定量。结果:硬脂酸镁中氯离子和硫酸根离子质量浓度分别在0.1~3.0和3~30μg·m L~(-1)范围内均呈良好线性关系,相关系数分别为0.999 7和0.999 8,平均回收率(n=9)分别为100.3%和100.4%,供试品溶液在24 h内稳定;171批样品中,氯离子含量为0.001%~0.107%,硫酸根离子含量为0.002%~1.467%。结论:该方法经方法学验证,可用于同时测定硬脂酸镁中的氯离子和硫酸根离子的含量,为其质量控制提供保证。
OBJECTIVE: To establish a method for simultaneous determination of chloride ion and sulfate ion in magnesium stearate by ion chromatography and to evaluate the quality status of chloride ion and sulfate ion ion in different grades of magnesium stearate. Methods: Dionex Ion Pac AS18 (4 mm × 250 mm) column and 10,40 mmol·L -1 potassium hydroxide eluent were used for gradient elution at a flow rate of 1.0 mL · min ~ (-1) ), Injection volume 25μL, standard curve method. RESULTS: The concentrations of chloride ion and sulfate ion in magnesium stearate showed good linearity in the range of 0.1-3.0 and 3-30 μg · m L -1, respectively, with correlation coefficients of 0.999 7 and 0.999 8, respectively. The average recoveries (n = 9) were 100.3% and 100.4%, respectively, and the stability of the test solution was stable within 24 h. In 171 samples, the chloride ion content was 0.001% ~ 0.107% and the sulfate ion content was 0.002% ~ 1.467 %. Conclusion: The method is validated by methodology and can be used for the simultaneous determination of chloride ion and sulfate ion in magnesium stearate to provide assurance for its quality control.