目的:建立一种离子色谱梯度淋洗抑制电导法快速测定尿液中草酸根、磷酸根及枸橼酸根离子浓度。方法:采集新鲜的尿样,经高速离心过0.2μm的微孔滤膜、On-Guard H小柱及C18预处理小柱后直接进样。选用Dionex IonPac AG23(50mm×4mm)阴离子保护柱和Dionex IonPac AS23(250mm×4mm)阴离子分析柱对样品进行分离,氢氧化钾溶液梯度淋洗,自再生抑制电导检测器检测。结果:线性范围为0.5~50μg·mL-1,r≥0.9998;日内精密度RSD≤3.6%,日间精密度RSD≤6.9%;样品加标平均回收率为96.0%~100.2%。结论:该方法操作简便、灵敏,选择性高,适用于常规样品分析。
Objective:To develop a simple method for the determination of oxalate,phosphate, citrate in human u- fine by ion chromatography with gradient elution and conductivity detection. Methods:Fresh collective urine sam- ples were centrifuged for 15 min at 5000 r · min -1 and then the above solution was filtered through a 0. 2 μm syr- inge membrane filter, On- Guard H column and C18 cleanup column before injection. The chromatographic separa- tion was performed on Dionex IonPac AG23 (50 mm× 4 mm) guard column, and an Dionex IonPac AS23 (250 mm × 4 mm) analytical column using potassium hydroxide as eluent with a serf - regeneration suppressor. Results: This novel method exhibited excellent regression( r 〉10. 9998 )in the range of 0. 5 -50μg·mL-1, satisfactory precision (RSD less than 3.6% within one day and less than 6. 9% day to day). The recovery obtained in the accuracy test was in the range of 96.0% - 100. 2%. Conclusion: The method is simple, accurate, stable and precise. It can be easily and conveniently adopted for the routine quality control analysis.