蔗糖及其有关物质含量的HPLC-CAD分析研究

目的：建立蔗糖及其有关物质含量的HPLC-CAD分析测定法。方法：采用Waters XBridge Amide色谱柱（4.6 mm×250 mm，3.5 μm），柱温为30℃；以乙腈-0.2%三乙胺水溶液（65：35）为流动相，流速为1.0 mL·min^-1；检测器为电喷雾检测器（CAD），雾化温度HIGH（50℃），幂率1.15，采样频率10 Hz，过滤常数5.0 s。结果：蔗糖与相邻杂质以及各杂质峰之间均达到基线分离；蔗糖质量浓度在4.95~99.08 μg·mL^-1及0.30~0.80 mg·mL^-1范围内线性关系良好（r>0.999），可分别用于有关物质检查和含量测定；检测下限为1.49 μg·mL^-1，定量下限为4.95 μg·mL^-1；进样精密度RSD为0.31%；重复性RSD为0.61%。4个批次的蔗糖样品含量均在99.09%~100.48%之间，有关物质含量在0.15%~0.25%之间。结论：所建方法专属、灵敏、耐用，操作简单，具有很好的应用前景。

Objective:To establish an HPLC-CAD method for the determination of sucrose and its related substances. Methods:The determination was carried out on a Waters XBridge Amide (4.6 mm×250 mm, 3.5 μm) column at 30℃, with acetonitrile-0.2% triethylamine solution (65:35) as mobile phase at a flow rate of 1.0 mL·min^-1.The detector of charged aerosol detector (CAD) was applied with at high nebulization temperature at 50℃ and collection frequency at 10 Hz with filter constant of 3.6 s, and PFV of 1.15.Results:Under the above chromatographic conditions, this method successfully achieved baseline separation among the peaks of sucrose, it's adjacent impurities and the other impurities obtained.The fine linear ranges of sucrose were between 4.95-99.08 μg·mL^-1 and 0.30-0.80 mg·mL^-1 with the correlation coefficients>0.999, suitable to the test of related substances and assay of sucrose, respectively.The LOD was 1.49 μg·mL^-1 and the LOQ was 4.95 μg·mL^-1.The RSDs of precision and repeatability were 0.31% and 0.61%, respectively.The contents of sucrose in four batches were all in the ranges of 99.09%-100.48%, and the total impurity was all in the ranges of 0.15%-0.25%.Conclusion:The established HPLC-CAD method is specific, sensitive, robust, and easy to operate with a promising prospect.

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