Determination of calcium， magnesium， fluorine and phosphate ions in human urineby solid phase extraction-ion chromatography
HAN Xiaoou, YU Bo, LIU Shunxin, CAO Zhongbo
Liaoning Center for Disease Control and prevention, Liaoning Key Laboratory of environment and population health monitoring,Shenyang 110005, China
摘要：建立固相萃取-离子色谱法测定人尿液中钙、镁两种阳离子和氟、磷酸根两种阴离子。采用C18固相萃取柱去除样品中杂质以消除干扰，以CS12 A型阳离子交换柱为分离柱，以甲基磺酸溶液为淋洗液，等度洗脱，测定钙、镁离子；以AS15型阴离子交换柱为分离柱，以KOH溶液为淋洗液，梯度洗脱，测定氟、磷酸根离子。钙、镁离子的质量浓度在0.25～10 mg/L范围内，氟、磷酸根离子的质量浓度分别在0.002 5～0.05 mg/L、1.25～50 mg/L范围内与色谱峰面积具有良好的线性关系，相关系数均大于0.999 0，方法检出限为0.002～0.2 mg/L。样品加标回收率为86.0%～99.5%，测定结果的相对标准偏差为0.12%～5.50%(n=6)。该方法操作简便，灵敏度高。
Abstract：A solid phase extraction-ion chromatography was established for the determination of calcium, magnesium cations, fluorine and phosphate anions in human urine. C18 solid phase extraction column was used to remove impurities in the sample to eliminate interference. CS12A cation exchange column was used as the separation column and methyl sulfonic acid solution was used as the eluent. Calcium and magnesium ions were determined by equal elution. Fluoride and phosphate ions were determined by gradient elution with AS15 anion exchange column as separation column and KOH solution as eluent. The mass concentrations of calcium and magnesium ions in the range of 0.25-10 mg/L, fluorine and phosphate ions in the range of 0.002 5-0.05 mg/L and 1.25-50 mg/L respectively had a good linear relationship with the chromatographic peak area, the correlation coef ficients were all more than 0.999 0, and the detection limit of the method was 0.002-0.2 mg/L. The recoveries of spiked samples were 86.0%-99.5%, and the relative standard deviations of the determination results were 0.12%-5.50%(n=6). The method is simple and sensitive.
Keywords：solid phase extraction; ion chromatography; urine; calcium ion; magnesium ion; fluorine ion; phosphateion
HAN Xiaoou，YU Bo，LIU Shunxin，et al. Determination of calcium，magnesium，fluorine and phosphate ions in human urine by solid phase extraction-ion chromatography[J]. Chemical Analysis and Meterage，2022，31(7)：48.