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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nifdc.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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离子色谱法测定达肝素钠中的亚硝酸根

Determination of nitrite in dalteparin sodium by ion chromatography

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出版年·卷·期(页码):2011,31 (11):0-0
DOI: 10.16155/j.0254-1793.2017.01.01
-----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100 μL,柱温30 ℃,电导检测器检测。 结果: 亚硝酸根检出限为1 μg·L-1,在25~1000 μg·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25~200 μg·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。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: A si mple,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 0.9997.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.

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