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[摘要]
目的 建立亲水作用色谱–蒸发光散射(HILIC-ELSD)法测定甲基纤维素中氯离子。方法 采用Thermo Acclaim Trinity P1 HILIC色谱柱(100 mm×3.0 mm,3μm);流动相:乙腈–20 mmol/L乙酸铵水溶液(60∶40)(乙酸调pH 5.0);体积流量:0.8 mL/min;柱温:30℃;进样量:10 μL;检测器漂移管温度105℃;氮气流量3.5 L/min。结果 氯离子在1~10 μg/mL与峰面积呈良好的对数线性关系,氯离子的最低检出质量浓度为0.5 μg/mL;平均回收率为99.4%,RSD值为1.6%。结论 此方法精密度好,回收率高,操作简单,能够准确测定甲基纤维素样品中的氯离子。
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[Abstract]
Objective To establish an HILIC-ELSD method for determination of chloridion in methylcellulose. Methods The separation was carried out on Thermo Acclaim Trinity P1 HILIC (100 mm×3.0 mm, 3 μm). The mobile phase was consisted of acetonitrile-20 mmol/L ammonium acetate solution (60:40, adjusted to pH 5.0 by acetic acid). The flow rate was 0.8 mL/min. The column temperature was 30℃, and volume of injection was 10 µL. The detector drift tube temperature was 105℃ and the nitrogen flow rate was 3.5 L/min. Results The linear relations was good between chloridion and peak area in the range of 1-10 μg/mL. The lowest detection concentration of chloride ion was 0.5 μg/mL. The average recovery rate was 99.4% with RSD value 1.6%. Conclusion The method has good precision, high recovery, and simple operation, which can accurately determine chloride ion content in methyl cellulose samples.
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