离子色谱法测定冰硼散中硫酸钠和氯化钠的含量
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摘要
目的建立离子色谱法测定冰硼散中硫酸钠和氯化钠含量的方法。方法采用Thermo Dionex IonPac AS11-HC离子交换色谱柱(250 mm×4 mm),Thermo Dionex IonPac AG11-HC保护柱(50 mm×4 mm),流动相为30mmol/L氢氧化钾溶液,等度洗脱,流速1.0 ml/min,柱温30℃;电导检测器,电导池温度35℃;进样量25μl。结果 10.0～100.0μg/ml范围内,硫酸根离子色谱峰峰面积与其浓度呈良好的线性关系(r=0.9997,n=6),平均回收率为100.6%;10.0～100.0μg/ml范围内,氯离子色谱峰峰面积与其浓度呈良好的线性关系(r=0.9998,n=6),平均回收率为102.6%。4家企业5批样品检出氯化钠,含量为0.19～0.44 g/g。结论本方法经方法学验证简便、快速、准确、重复性好,可用于冰硼散中硫酸钠、氯化钠的质量控制。
Objective To establish an ion chromatography method for determination of the contents of sodium sulfate and sodium chloride in Bingpeng San. Methods The chromatographic column was Thermo Dionex IonPac AS11-HC(250 mm×4 mm); the protected column was Dionex IonPac AG11-HC(50 mm×4 mm); the isocratic elution was performed, using 30 mmol/L potassium hydroxide solution as mobile phase; the ?ow rate was 1.0 ml/min, the column temperature was 30 ℃, the electrical conductivity cell temperature was 35 ℃, and the injection volume was25 μl. Results In the range of 10.0-100.0 μg/ml, the peak area of sulfate ion had a good linear relationship with its concentration(r=0.9997, n=6), and the average recovery was 100.6 %. In the range of 10.0-100.0 μg/ml, the peak area of chloride ion had a good linear relationship with its concentration(r=0.9998, n=6), with an average recovery of102.6 %. Sodium chloride was detected in 5 batches of samples from 4 factories. The content of sodium chloride was in the range of 0.19-0.44 g/g. Conclusion The established method in this study is simple, convenient and rapid, with high accuracy and precision. It can be used for quality control of sodium sulfate and sodium chloride in Bingpeng San.
Objective To establish an ion chromatography method for determination of the contents of sodium sulfate and sodium chloride in Bingpeng San. Methods The chromatographic column was Thermo Dionex IonPac AS11-HC(250 mm×4 mm); the protected column was Dionex IonPac AG11-HC(50 mm×4 mm); the isocratic elution was performed, using 30 mmol/L potassium hydroxide solution as mobile phase; the ?ow rate was 1.0 ml/min, the column temperature was 30 ℃, the electrical conductivity cell temperature was 35 ℃, and the injection volume was25 μl. Results In the range of 10.0-100.0 μg/ml, the peak area of sulfate ion had a good linear relationship with its concentration(r=0.9997, n=6), and the average recovery was 100.6 %. In the range of 10.0-100.0 μg/ml, the peak area of chloride ion had a good linear relationship with its concentration(r=0.9998, n=6), with an average recovery of102.6 %. Sodium chloride was detected in 5 batches of samples from 4 factories. The content of sodium chloride was in the range of 0.19-0.44 g/g. Conclusion The established method in this study is simple, convenient and rapid, with high accuracy and precision. It can be used for quality control of sodium sulfate and sodium chloride in Bingpeng San.
引文
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[11]张元,李伟青,周伟娥,等.离子色谱法同时测定丹参注射剂中6种无机阴离子[J].中国实验方剂学杂志, 2015, 21(17):24-27.
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[2]朱雪妍.离子色谱法测定血栓通注射液中辅料氯化钠和枸橼酸钠的含量[J].药物分析杂志, 2015, 35(7):1236-1239.
[3]任华忠,封家福,伍朝君.离子色谱法测定注射用硫代硫酸钠中的亚硫酸盐和硫酸盐[J].华西药学杂志, 2015, 30(1):103-104.
[4]常欣.离子色谱法测定芒硝中硫酸根的含量[J].海峡药学,2016, 28(10):60-61.
[5]赵晶晶.离子色谱法测定Na3PO4·12H2O中的杂质Cl-和SO42-的含量[J].分析仪器, 2018,(1):57-62.
[6]唐静,闫海涛,王鑫光.离子色谱法测定土壤中氯离子、硫酸根离子、硝酸根离子[J].化学分析计量, 2017, 26(3):57-60.
[7]王宇,黄勇.离子色谱法同时检测利咽灵片中9种无机阴离子[J].中药材, 2017, 40(10):2380-2382.
[8]谢玉惠,龙兴浩.离子色谱法同时测定附子理中丸中9种无机阴离子含量[J].安徽医药, 2016, 20(8):1490-1494.
[9]粟贵,刘雁鸣,龙海燕,等.离子色谱法测定羟苯乙酯中氯离子和硫酸根离子及不同级别产品质量状况的评价[J].中国药师,2017, 20(8):1367-1370.
[10]周伟娥,杨立佼,谢巍,等.离子色谱法同时测定感冒清热颗粒中9种无机阴离子[J].中国药房, 2015, 26(18):2546-2549.
[11]张元,李伟青,周伟娥,等.离子色谱法同时测定丹参注射剂中6种无机阴离子[J].中国实验方剂学杂志, 2015, 21(17):24-27.
[12]徐桂连,耿欣.离子色谱法测定碳酸锂原料药中的氯化物及硫酸盐[J].中国药师, 2015, 18(2):324-326.