School of Basic Medicine, Southern Medical University, Guangzhou 510515, China.
Hygiene Detection Center, Guangdong Provincial Key Laboratory of Tropical Disease Research, School of Public Health, Southern Medical University, Guangzhou 510515, China.
J Pharm Biomed Anal. 2019 Jan 30;163:58-63. doi: 10.1016/j.jpba.2018.09.030. Epub 2018 Sep 19.
A fast, precise, and accurate method that can simultaneously determine 7 anions in whole blood was established by on line dialysis-double suppression ion chromatography. Performance parameters which could affect the determination of anions were optimized, including the selection of protein precipitant in samples, the amount of filtrate discarded, selection of eluent flow rate, influence of the Ag-Na column on experimental results, influence of ethylenediamines on ClO, and investigation of nitrogen drying. Finally, 3.6 mmol/L sodium carbonate was selected as eluent, with a flow rate of 0.8 mL/min, to separate the 7 anions. Blood and alcohol (v/v, 1:4) were used to precipitate the proteins in blood. The 7 anions reached an adequate recovery rate when the first 2 mL of filtrate from the C18 column was discarded. The recovery rate at LLOQ, low, medium, and high concentrations was 80-120%. The correlation coefficients (r) of the calibration curves of the targeted anions ranged from 0.9975 to 0.9998. The limit of detection (LOD) was 0.309-7.71 μg/L. This method has simple pretreatment, high accuracy, and good reproducibility and selectivity, and is suitable for the separation and determination of anions in blood.
建立了一种在线透析-双抑制离子色谱法,可同时测定全血中的 7 种阴离子。优化了可影响阴离子测定的性能参数,包括样品中蛋白质沉淀剂的选择、滤液丢弃量、洗脱液流速的选择、Ag-Na 柱对实验结果的影响、乙二胺对 ClO 的影响以及氮干燥的研究。最终选择 3.6mmol/L 碳酸钠作为洗脱液,流速为 0.8mL/min,以分离 7 种阴离子。血液和酒精(v/v,1:4)用于沉淀血液中的蛋白质。当从 C18 柱丢弃前 2mL 滤液时,7 种阴离子达到足够的回收率。LLOQ、低、中、高浓度的回收率为 80-120%。目标阴离子校准曲线的相关系数(r)范围为 0.9975 至 0.9998。检测限(LOD)为 0.309-7.71μg/L。该方法预处理简单,准确度高,重现性和选择性好,适用于血液中阴离子的分离和测定。