热能分析仪测定那屈肝素钙中的N-NO含量  

Determination of N-NO in Nadroparin Calcium by Thermal Energy Analyzer

作　　者：赵焕荣[1] 马志华[1] 杜旭召[1] 姬胜利[1] 

机构地区：[1]河北常山生化药业股份有限公司,河北石家庄050800

出　　处：《食品与药品》2013年第6期384-386,共3页Food and Drug

摘　　要：目的 建立那屈肝素钙中N-NO含量测定方法.方法 采用热能分析仪（TEA）进行分析.运行参数：氮气压力5 psi,氮气流量35 mL/min,冷却液温度0～5℃,液滴回流速率1～2 s/滴,氧气压力2 psi,灵敏度235,进样量50 μL.结果 N-NO含量以N-亚硝基二正丙胺（NDPA）含量计,NDPA浓度在0.03～0.15 μg/mL范围内线性关系良好,相关系数r=0.9991;精密度试验（n=6）的相对标准偏差（RSD）为2.27％;定量限（信噪比10：1）和检测限（信噪比3：1）分别为0.03和0.005 μg/mL：此法的平均加样回收率为99.75％,RSD为0.93％.结论 本实验得到的方法精密度好,准确度高,适合那屈肝素钙中N-NO的含量测定.Objective To establish the method for determination of N-NO in nadroparin calcium.Methods Thermal energy analyzer was used; the operating parameters were as follows：nitrogen pressure：5 psi; nitrogen flow rate：35 mL/min; coolant temperature：0～5 ℃; droplet reflux rate：1～2 s/drop; oxygen pressure：2 psi; sensitivity：235; injection volume：50 μL.Results The content of N-NO was calculated as the content of N-nitrosodipropylamine （NDPA）,the linear range of NDPA was 0.03～0.15 μg/mL,r=0.9991; RSD of precision （n=6） was 2.27 ％; the limit ofquantitation （S/N=10：1） was 0.03 μg/mL,and the limit of detection （S/N=3：1） was 0.005 μg/mL.The average recovery （n=9） was 99.75 ％,with RSD of 0.93 ％.Conclusion The established method had good precision,accuracy,and is suitable for the determination of N-NO in nadroparin calcium.

关 键 词：N-NO 那屈肝素钙 热能分析仪 

分 类 号：TQ460.72[医药卫生—药物分析学]