山东化工2024,Vol.53Issue(23) :185-188.

高效液相色谱法测定头孢他啶中甲酸、乙酸含量

Determination of Formic Acid and Acetic Acid in Ceftazidime by HPLC

崔成伟 李蕊 刘姣 郑宏杰 王喃喃
山东化工2024,Vol.53Issue(23) :185-188.

高效液相色谱法测定头孢他啶中甲酸、乙酸含量

Determination of Formic Acid and Acetic Acid in Ceftazidime by HPLC

崔成伟 1李蕊 1刘姣 1郑宏杰 1王喃喃1
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作者信息

  • 1. 山东鲁抗医药股份有限公司,山东济宁 272000
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摘要

目的:建立测定头孢他啶中甲酸、乙酸含量的反相高效液相色谱法.方法:采用反相高效液相色谱法,色谱柱以十八烷基硅烷键合硅胶为填充剂(Agilent ZORBAX SB-Aq C18,250 mm×4.6 mm,5 μm),流动相A为0.7%磷酸水-甲醇(95∶5,体积比),流动相B为甲醇,梯度洗脱,流速为1.2mL/min,柱温为30 ℃,检测波长为210 nm.结果:甲酸、乙酸峰间的分离度大于1.5.甲酸定量限为20×10-6(相当于样品浓度的百分比为0.02%),乙酸定量限为40×10-6(相当于样品浓度的百分比为0.04%),甲酸检测限为2×10-6(相当于样品浓度的百分比为0.002%),乙酸检测限为4×10-6(相当于样品浓度的百分比为0.004%).甲酸在0.047 9~0.718 1 mg/mL质量浓度范围内,线性方程为 y=1.604 3x+0.009 4,r=0.999 5>0.990,乙酸在0.049 6~0.743 7 mg/mL 质量浓度范围内,线性方程为 y=0.930 1x+0.008 5,r=0.997 3>0.990.甲酸的回收率为104.4%~116.2%,乙酸的回收率为93.8%~99.9%.结论:该分析方法容易操作、专属性好、准确度高、灵敏度高,能够快速并有效地检出头孢他啶中甲酸、乙酸的含量.

Abstract

Objective:To establish an RP-HPLC method for the determination of formic acid and acetic acid in ceftazidime.Methods:RP-HPLC was used.The chromatographic column is Agilent ZORBAX SB Aq C18,250 mm × 4.6 mm,5 μm.The mobile phase A is 0.7%phosphoric acid water-methanol(95∶5,volume ratio),the mobile phase B is methanol with gradient elution.The flow rate is 1.2 mL per minute,the column temperature is 30℃,and the detection wavelength is 210 nm.Results:The separation degree between formic acid and acetic acid peaks is greater than 1.5.The LOQ of formic acid is 20 × 10-6(equivalent to a percentage of sample concentration of 0.02%),the LOQ of acetic acid is 40 × 10-6(equivalent to a percentage of sample concentration of 0.04%),the LOD for formic acid is 2×10-6(equivalent to a percentage of sample concentration of 0.002%),the LOD for acetic acid is 4×10-6(equivalent to a percentage of sample concentration of 0.004%).The linear equation for formic acid in the concentration range of 0.047 9~0.718 1 mg/mL is y=1.604 3x+0.009 4,r=0.999 5>0.99,and for acetic acid in the concentration range of 0.049 6~0.743 7 mg/mL,y=0.930 1x+0.008 5,r=0.997 3>0.99.The recovery rate of formic acid is 104.4%~116.2%,and the recovery rate of acetic acid is 93.8%~99.9%.Conclusion:This analytical method is easy to operate,has good specificity,high accuracy,and high sensitivity,and can quickly and effectively detect the content of formic acid and acetic acid in ceftazidime.

关键词

头孢他啶/甲酸/乙酸/高效液相色谱法

Key words

ceftazidime/formic acid/acetic acid/HPLC

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出版年

2024
山东化工
山东省化工研究院 山东省化工信息中心

山东化工

影响因子:0.249
ISSN:1008-021X
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