摘要
目的:建立并优化一种简单、快速、高灵敏度、重现性好的离子色谱法测定达肝素钠中残留的亚硝酸根含量。方法:达肝素钠制成40 mg.mL-1的溶液,加9倍体积乙醇沉淀,离心后取上层清液过滤后直接进样。分离使用IonPac AS19分析柱和保护柱,淋洗液为20 mmol.L-1氢氧化钠,流速1.0 mL.min-1。AMMS 300膜抑制器,化学抑制,再生液为25 mmol.L-1硫酸。进样量100μL,柱温30℃,电导检测器检测。结果:亚硝酸根检出限为1μg.L-1,在25～1000μg.L-1浓度范围内,相关系数0.9997,平行试验RSD小于4%,加标浓度为25～200μg.L-1亚硝酸根,方法回收率为98.5%～107.9%。结论:本实验得到的方法灵敏度高,回收率好,重现性好,利于延长色谱柱寿命。本方法可用于达肝素钠的质量控制,也为其他多糖类化合物中阴离子测定提供参考。
Objective： A simple,rapid,reliable and high sensitive ion chromatographic method was established and improved for determination of nitrite in low - molecular - weight heparin. Methods： Ethanol was added in dalteparin sodium solution. The suspension was centrifuged and filtered. Filtrate was injected to IC. Separation was performed on Ion Pac AS19 column,equipped with a guard column of the same material. The eluent was 20mmol · L^-1 NaOH. The column temperature was maintained at 30 ℃. Conductivity detector and AMMS 300 membrane suppressor was used and regenerant solution was 25 mmol· L^-1 H2SO4. The flow rate and sample volume injected were 1 mL ·min^-1 and 100 μL,respectively. Results： Detection limit of nitrite was 1 μg · L^-1. The calibration curve of nitrite was linear in the concentration range of 25 - 1000 μg · L^-1 and the coefficient was O. 9997. The RSD of parallel tests did not exceed 4%. The average recovery of the described method was 98.5% - 107.9% spiked with 25 -200 μg · L^-1 nitrite. Conclusions： The new method could protect the separation column and obtain high reproducibility. Consequently,it was more suitable to determine nitrite content in dalteparin sodium.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2011年第11期2171-2173,共3页
Chinese Journal of Pharmaceutical Analysis
关键词
低分子肝素
达肝素钠
亚硝酸根
离子色谱法
low - molecular to determine nitrite content in dalteparin sodium - weight heparin
daheparin sodium
nitrite
ion chromatography
