Simultaneous determination of ceftazidime and avibactam in patients by isocratic ion-pair liquid chromatography with photometric detection

IF 3.2

Journal of chromatography open Pub Date : 2025-03-11 DOI:10.1016/j.jcoa.2025.100212

Constantin Lier , Frieder Kees , Andrea Witowski , Tim Rahmel , Steffen Pockes , Christoph Dorn

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Abstract

A simple and fast HPLC-UV method is described for the simultaneous determination of total or free ceftazidime and avibactam in serum, which is suitable for therapeutic drug monitoring (TDM) or pharmacokinetic studies in man. Sufficient retention of the very polar avibactam was obtained by addition of tetrabutylammonium hydrogen sulfate (TBA) as ion pairing agent, thus allowing the determination of both drugs in serum by isocratic elution. Total concentrations were determined after protein precipitation with acetonitrile, free concentrations after ultrafiltration. Separation was performed using an XBridge BEH C18 column with a mobile phase consisting of 20 mM sodium phosphate buffer/acetonitrile 90:10 (v/v), pH 6.5, containing 5 mM TBA. The lower limit of quantification was 1 mg/L for ceftazidime and 0.5 mg/L for avibactam, respectively. The imprecision of the determination of total drug was <3 %, the accuracy between 99.0 % and 104 %. Determination of free drug in quality control samples resulted in unbound fractions of 97.9 ± 2.0 % for ceftazidime and 99.4 ± 3.2 % for avibactam.

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等密度离子对液相色谱-光度法同时测定头孢他啶和阿维巴坦的含量

建立了同时测定血清中总头孢他啶和游离头孢他啶和阿维巴坦含量的高效液相色谱-紫外分光光度法，适用于人体治疗药物监测或药代动力学研究。通过添加四丁基硫酸氢铵（TBA）作为离子配对剂，获得极极性阿维巴坦的充分保留，从而允许用等压洗脱法测定血清中的两种药物。乙腈沉淀后测定总浓度，超滤后测定游离浓度。采用XBridge BEH C18色谱柱进行分离，流动相为20 mM磷酸钠缓冲液/乙腈90:10 (v/v), pH 6.5，含5 mM TBA。头孢他啶的定量下限为1 mg/L，阿维巴坦的定量下限为0.5 mg/L。总药含量测定的不精密度为3%，准确度在99.0% ~ 104%之间。品控样品中游离药物的测定结果表明，头孢他啶和阿维巴坦的分离率分别为97.9%±2.0%和99.4%±3.2%。

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