胶束电动毛细管电泳在线富集结合离线选择性萃取用于硫酸软骨素的灵敏分析。
Offline Selective Extraction Combined with Online Enrichment for Sensitive Analysis of Chondroitin Sulfate by Capillary Electrophoresis.
机构信息
School of Pharmaceutical Sciences, Cheeloo College of Medicine, Shandong University, Jinan, Shandong 250012, China.
School of Chemistry and Chemical Engineering, Qilu University of Technology, Jinan 250353, China.
出版信息
J Chromatogr Sci. 2020 Sep 29;58(9):868-874. doi: 10.1093/chromsci/bmaa052.
A capillary electrophoresis (CE) method combined with online and offline enrichment for improving the detection sensitivity of chondroitin sulfate (CS) is established. The online enrichment method is based on the field-amplified sample stacking and large volume electrokinetic injection, and offline enrichment is based on the association between cetyltrimethylammonium chloride and CS. Experimental parameters affecting CE method such as the type and pH of background electrolyte, the injection mode and time and the steps of offline enrichment were optimized. Under optimum conditions, the calibration plot between CS concentration and peak area was linear in the range of 1 ~ 100 μg/mL. The enrichment factor was 130 times and the limit of detection was 50 ng/mL. The average recovery was 103.5% and the relative standard deviation of peak area was <2.0%. The method was successfully applied to the quantitative analysis of CS in drugs.
建立了一种毛细管电泳（CE）方法，结合在线和离线富集，以提高硫酸软骨素（CS）的检测灵敏度。在线富集方法基于场放大样品堆积和大体积电动进样，离线富集基于十六烷基三甲基氯化铵与 CS 的缔合。优化了影响 CE 方法的实验参数，如背景电解质的类型和 pH 值、进样模式和时间以及离线富集的步骤。在最佳条件下，CS 浓度与峰面积之间的校准曲线在 1 ～ 100 μg/mL 范围内呈线性。富集因子为 130 倍，检测限为 50 ng/mL。平均回收率为 103.5%，峰面积的相对标准偏差小于 2.0%。该方法成功应用于药物中 CS 的定量分析。
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