重症感染患者亚胺培南检测方法的建立及临床应用
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篇名: 重症感染患者亚胺培南检测方法的建立及临床应用
TITLE: Establishment and clinical application of imipenem measurement method in patients with severe infection
摘要: 目的 建立适用于检测重症感染患者亚胺培南血药浓度的二维液相色谱法,并应用于临床。方法基于全自动二维液相色谱仪建立亚胺培南血药浓度检测方法,以一维色谱柱AstonSNCB(50mm×4.6mm,5μm)萃取分离目标物,再经二维色谱柱AstonSCB(250mm×4.6mm,5μm)进一步分离测定。一维流动相为亚胺培南-1D移动相[乙腈-甲醇-水(15∶10∶75,V/V/V)],流速为1.0mL/min;二维流动相为72%OPI-1有机移动相(色谱级甲醇)-20%BPI-1碱性移动相[水(含20.0mmol/L的磷酸铵,用三乙胺调pH至7.2)]-8%API-1酸性移动相[水(含20.0mmol/L的磷酸铵,用磷酸调pH至3.0)],流速为1.0mL/min;柱温为40℃,紫外检测波长为310nm,进样量为100μL。洗脱程序:0~3.40min,一维色谱柱(亚胺培南-1D移动相);3.40~11.00min,二维色谱柱(72%OPI-1有机移动相-20%BPI-1碱性移动相-8%API-1酸性移动相)。结果亚胺培南检测质量浓度的线性范围为0.171~18.570μg/mL(R2=0.9999),定量下限为0.171μg/mL;回收率在93.47%~106.16%(n=5),日内和日间精密度的RSD均低于15%(n=5)。51例患者的亚胺培南谷浓度为0~19.57μg/mL。结论所建立的方法前处理简单、快捷,进样量大,可用于重症感染患者亚胺培南血药浓度的检测。
ABSTRACT: OBJECTIVE To establish two-dimensional liquid chromatography method for the determination of imipenem blood concentration and apply it in clinical practice. METHODS The method for the determination of imipenem blood concentration was established based on automatic two-dimensional liquid chromatography. The targets were extracted by 1-dimensional column Aston SNCB (50 mm ×4.6 mm, 5 μm) and further separated and determined by 2-dimensional column Aston SCB (250 mm×4.6 mm, 5 μm). The 1-dimensional mobile phase was imipenem-1D mobile phase [acetonitrile-methanol-water (15∶10∶75, V/V/V)] with a flow rate of 1.0 mL/min; 2-dimensional mobile phase was 72%OPI-1 organic mobile phase (chromatographic grade methanol)-20% BPI-1 alkaline mobile phase [water (containing 20.0 mmol/L ammonium phosphate, pH adjusted to 7.2 with triethylamine)]-8%API-1 acidic mobile phase [water (containing 20.0 mmol/L ammonium phosphate, pH adjusted to 3.0 with phosphoric acid)] with a flow rate of 1.0 mL/min; the column temperature was 40 ℃, UV detection wavelength was 310 nm and injection volume was 100 μL. Elution procedure: 1-dimensional column consisted of imipenem-1D mobile phase with eluting for 0-3.40 min; 2-dimensional column consisted of 72% OPI-1 organic mobile phase-20%BPI-1 alkaline mobile phase-8%API-1 acidic mobile phase with eluting for 3.40-11.00 min. RESULTS The linear range of imipenem was 0.171-18.570 μg/mL (R 2=0.999 9) with the lower limit of quantification for 0.171 μg/mL; the recovery rate ranged from 93.47% to 106.16%( n=5) and the RSDs of both intra-day and inter- day precision were below 15% (n=5). The minimum concentration of imipenem in 51 patients ranged from 0 to 19.57 μg/mL. CONCLUSIONS The established method is simple and fast with the large scale of sample, and can be used for the imipenem blood concentration monitoring in patients with severe infection.
期刊: 2024年第35卷第16期
作者: 陈永妍;孙迪迪;韩文超;王前;张寒娟
AUTHORS: CHEN Yongyan,SUN Didi,HAN Wenchao,WANG Qian,ZHANG Hanjuan
关键字: 亚胺培南;血药浓度监测;重症感染;二维液相色谱
KEYWORDS: imipenem; blood concentration monitoring; severe infection; 2D-LC/UV
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