离子色谱法同时测定药品中巴比妥酸和硝酸盐  

Simultaneous determination of barbituric acid and nitrate in pharmaceuticals by ion chromatography

作　　者：潘忠全 黄选忠 PAN Zhongquan;HUANG Xuanzhong(Prevention and Health Protection Centre of Hubei Yuanan County,Yuanan 444200,China;Prevention and Health Protection Centre of Hubei Xingshan County,Xingshan 443700,China)

机构地区：[1]湖北远安县疾病预防控制中心,湖北远安444200 [2]湖北兴山县疾病预防控制中心,湖北兴山443700

出　　处：《化学分析计量》2022年第9期41-45,共5页Chemical Analysis And Meterage

摘　　要：建立离子色谱–抑制电导检测法同时测定巴比妥酸和硝酸盐的分析方法。以SH-AC-3型阴离子交换柱为分离柱,以5.0 mmol/L NaCO溶液为淋洗液,流量为1.0 mL/min,采用等度洗脱的方式将巴比妥酸和硝酸盐与氟化物、氯化物、磷酸盐和硫酸盐等常见阴离子完全分离,通过抑制电导检测。巴比妥酸的质量浓度在0.10~50.0 mg/L范围内与色谱峰面积具有良好的线性关系,线性相关系数为0.999 9;硝酸盐的质量浓度在0.10~50.0 mg/L范围内与色谱峰面积具有良好的线性关系,线性相关系数为0.999 3。巴比妥酸和硝酸盐的检出限分别为0.10 mg/L和0.03 mg/L,加标回收率分别为90.4%~101.4%和98.0%~101.3%,5次平行测定结果的相对标准偏差分别为1.71%~2.39%和1.21%~2.66%。该方法操作简便、快速,可用于巴比妥、苯巴比妥和维生素B12等样品中巴比妥酸和硝酸盐的定量分析。A new method for simultaneous determination of barbituric acid and nitrate by ion chromatography with suppressed conductivity detection was developed.SH-AC-3 anion exchange column was used as separation column,5.0 mmol/L NaCOsolution was used as eluent and the flow rate was 1.0 mL/min,barbituric acid and nitrates were completely separated from common anions such as fluoride,chloride,phosphate and sulfate by isometric elution,and were detected by inhibiting conductance.There was a good linear relationship between the chromatographic peak area and the concentration of barbituric acid in the range of 0.10–50.0 mg/L with the correlation coefficient of 0.999 9,the chromatographic peak area of nitrate had good linear relationship with its concentration in the range of 0.10–50.0 mg/L,and the correlation coefficients were 0.999 3.The detection limits of barbituric acid and nitrate were 0.10 mg/L and 0.03 mg/L respectively,and the recoveries of spiked samples were 90.4%–101.4% and 98.0%–101.3% respectively,the relative standard deviations of the five parallel determination results were 1.71%–2.39% and 1.21%–2.66% respectively.The method issimple and fast,and it can be used for the barbituric acid and nitrate quantitative analysis of barbiturate,phenobarbital and vitamin B12.

关 键 词：离子色谱法 巴比妥酸 硝酸盐 巴比妥 苯巴比妥 维生素B12 药品 

分 类 号：O657.7[理学—分析化学]