摘要
目的建立离子色谱法测定单硝酸异山梨酯片剂中硝酸盐和亚硝酸盐的残留。方法采用20 mmol·L^-1氢氧化钾溶液为淋洗液进行洗脱,以Dionex IonPac ASⅡ-HC(4 mm×250 mm)色谱柱以及Dionex IonPac ASⅡ-HC(4 mm×50 mm)保护柱进行分离,流速为1.0 mL·min^-1,ASRS 300 4-mm型连续自动再生阴离子抑制器和电导检测器抑制并检测,抑制电流为50 mA,电导池温度为30℃,进样量为25 μL。结果硝酸根离子、亚硝酸根离子与其他成分的分离度良好,硝酸根离子与亚硝酸根离子均在0.1~20 μg·mL^-1与测定值线性关系良好,其检测限均为0.01 μg·mL^-1,定量限均为0.03 μg·mL^-1,平均回收率分别在91.7%~97.9%和93.5%~96.6%。结论本方法灵敏度高,专属性强,准确可靠,适用于单硝酸异山梨酯片剂中硝酸盐和亚硝酸盐的检测。
Objective To determine nitrate and nitrite residues in isosorbide mononitrate preparations by ion chromatography.Methods The determination was performed on an Dionex IonPac ASⅡ-HC (4 mm×250 mm) column with a Dionex IonPac ASⅡ-HC (4 mm×50 mm) guard column.The drenching solution was 20 mmol·L^-1 potassium hydroxide solution,and the flow rate was 1.0 mL·min^-1.The nitrate and nitrite were detected by suppressed conductivity with an ASRS 300 4-mm suppressor at a current of 50 mA,the temperature of conductivity cell was 30℃,and the injection volume was 25 μL.Results The nitrate,nitrite and other ions were well separated.The nitrate and nitrite calibration curves showed good linearity at 0.1~20 μg·mL^-1,the limit of detection was 0.01 μg·mL^-1,and the limit of quantification was 0.03 μg·mL^-1.The average recoveries of the two ions were at 91.7%~97.9% and 93.5%~96.6%,respectively.Conclusion The method is highly sensitive and specific,which can be used to determine nitrate and nitrite residues in isosorbide mononitrate preparations.
作者
段书涛
张磊
DUAN Shu-tao;ZHANG Lei(Linyi Inspection and Testing Center,Linyi Shandong 276000;ShandongCenter for Food and Drug Evaluation&Certification,Jinan 250014)
出处
《中南药学》
CAS
2020年第11期1888-1891,共4页
Central South Pharmacy
基金
2019年度山东省药品质量安全风险监测项目。
