离子色谱法测定木糖醇中氯离子、硫酸根离子和磷酸根离子及不同级别产品质量状况的评价
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摘要
目的建立离子色谱法同时测定木糖醇中氯离子、硫酸根离子和磷酸根离子的含量,并评价不同级别木糖醇中氯离子、硫酸根离子和磷酸根离子含量的质量状况。方法采用Dionex IonPac AS19阴离子分析柱(4 mm×250 mm,5μm),以氢氧化钾为淋洗液梯度洗脱,流速为1.0 mL·min~(-1),标准曲线法测定。样品用超纯水溶解并稀释后直接进样。结果氯离子、硫酸根离子和磷酸根离子分别在0.01~2.0μg·mL~(-1)、0.02~6.0μg·mL~(-1)、0.05~4.0μg·m L~(-1)内线性关系良好,r分别为0.9998、0.9995和0.9995;加样回收率(n=6)分别为96.4%、93.8%、99.3%,RSD分别为1.6%、3.2%、1.4%。结论本方法操作简便、灵敏、高效,可用于同时测定木糖醇中氯离子、硫酸根离子和磷酸根离子的含量,为其质量控制提供保证。
Objective To establish an ion chromatography method to determine the content of chloride ion, sulfate ion and phosphate ion in xylitol, and to evaluate the content and quality of chloride ion, sulfate ion and phosphate ion in different levels of xylitol. Methods Dionex IonPac AS19(4 mm×250 mm, 5 μm) was used and potassium hydroxide was used as the mobile phase with gradient elution. The flow rate was 1.0 mL·min-1, and the quantitative method was standard curve. Samples were diluted with pure water followed by direct injection. Results The method showed good linearity at 0.01-2.0 μg·mL~(-1) for chloride ion(r = 0.9998), 0.02-6.0 μg·mL~(-1) for sulfate ion(r = 0.9995), and 0.05-4.0 μg·m L~(-1) for phosphate ion(r = 0.9995), respectively. The average recoveries(n = 6) were 96.4%(RSD = 1.6%), 93.8%(RSD = 3.2%) and 99.3%(RSD = 1.4%) for chloride ion, sulfate ion and phosphate ion, respectively. Conclusion The method is simple, sensitive and efficient, which can be used to determine the content of chloride ion, sulfate ion and phosphate ion in xylitol, and to control its quality.
Objective To establish an ion chromatography method to determine the content of chloride ion, sulfate ion and phosphate ion in xylitol, and to evaluate the content and quality of chloride ion, sulfate ion and phosphate ion in different levels of xylitol. Methods Dionex IonPac AS19(4 mm×250 mm, 5 μm) was used and potassium hydroxide was used as the mobile phase with gradient elution. The flow rate was 1.0 mL·min-1, and the quantitative method was standard curve. Samples were diluted with pure water followed by direct injection. Results The method showed good linearity at 0.01-2.0 μg·mL~(-1) for chloride ion(r = 0.9998), 0.02-6.0 μg·mL~(-1) for sulfate ion(r = 0.9995), and 0.05-4.0 μg·m L~(-1) for phosphate ion(r = 0.9995), respectively. The average recoveries(n = 6) were 96.4%(RSD = 1.6%), 93.8%(RSD = 3.2%) and 99.3%(RSD = 1.4%) for chloride ion, sulfate ion and phosphate ion, respectively. Conclusion The method is simple, sensitive and efficient, which can be used to determine the content of chloride ion, sulfate ion and phosphate ion in xylitol, and to control its quality.
引文
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[9]陆克平. 30%亚硫酸氢钠溶液样品中Cl-和SO42-的同时测定[J].色谱,2005,23(3):205-207.
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[2]任鸿均.木糖醇的生产新技术及其应用[J].化工科技市场,2005,(2):1-6.
[3]朱宏阳,周剑,李泳宁,等.木糖醇生产的研究进展[J].海峡药学,2012,24(5):5-7.
[4]姚静.药用辅料应用指南[M].北京:中国医药科技出版社,2011:205-206.
[5]杨柳,赵聪,姚默,等.木糖醇应用及毒副作用研究进展[J].安徽农业科学,2011,39(34):21355-21356.
[6]成英,闫书磊,明立雪.木糖醇的生产工艺及应用研究进展[J].甘肃石油和化工,2008,(3):18-21.
[7]王关斌,赵光辉.木糖醇的生产与发展趋势[J].浙江化工,2005,36(2):25-26.
[8]粟贵,刘雁鸣,龙海燕,等.离子色谱法测定药用辅料硬脂酸镁中氯离子和硫酸根离子及不同级别产品含量比较[J].药物分析杂志,2016,36(12):2251-2256.
[9]陆克平. 30%亚硫酸氢钠溶液样品中Cl-和SO42-的同时测定[J].色谱,2005,23(3):205-207.
[10]中国药典2015年版.四部[S]. 2015:479-480.
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