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出 处:《中国实验方剂学杂志》2014年第14期61-64,共4页Chinese Journal of Experimental Traditional Medical Formulae
基 金:广东省医学科学技术研究基金项目(A2012155)
摘 要:目的:建立测定维生素B。注射液中EDTA及硝酸根离子含量的离子色谱法。方法:采用lonPacAS11-Hc色谱柱(4.0mm×250mm),IonPacAS11-HCguard保护柱(4.0mm×50mm)和ASRS300抑制器(4mm),淋洗液为12mmol·L^-1氢氧化钠,流速1.0mL·min^-1,抑制电流60mA,电导检测器温度35℃,柱温30℃,进样体积25μL。结果:EDTA和硝酸根离子检出限分别为0.29,0.01mg·L^-1,EDTA在1.19~23.8mg·L^-1,线性关系良好(r=0.9997),回收率为98.2%.100.6%;硝酸根离子在1.0~10.0mg·L^-1线性关系良好(r=0.9996),回收率为97.9%~99.5%。结论:该实验方法选择性高,灵敏度好,测定结果准确,并且简便,快速,可用于注射液中ETDA及硝酸根离子的测定研究和质量控制。Objective: To develop a method by ion chromatography with suppressed conductivity detection for the determination of EDTA and nitrate ion in vitamin B1 injection. Method: Chromatographicseparation was achieved on an IonPac AS 11-HC column (4.0 mm × 250 mm) with an IonPac AS 11-HC guard column (4.0 mm x50 mm) and an ASRS 300 suppressor (4 ram). The eluent was 12 mmol ·L^-1 NaOH with flow rate 1.0 mL ·min ^-1 The suppressor current was 60 mA, and the conductivity detector temperature was set at 35 ℃ while the column temperature was maintained at 30 ℃. The injection volume was 25 μL. Result: The limit of determination of EDTA and nitrate ion were 0.29 mg ·L^-1 and 0.01 mg·L^-1 respectively. The standard curve of EDTA was linear in the concentration range of 1. 19-23.8 mg ·L^-1 and the correlation coefficient was 0. 999 7. The recoveries of the EDTA were between 98.2%-100.6%. The standard curve of nitrate ion was linear in the concentration range of 1.0-10.0 mg·L^-1 and the correlation coefficient was 0. 999 6. The recoveries of the nitrate ion were between 97.9%-99.5%. Conclusion: The proposed method shows high selectivity, sensitivity and good results. It is proved to be rapid and convenient. It can be employed for the quality control and research of EDTA and nitrate ion in injection products.
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