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胶束电动毛细管色谱法-紫外检测法与液相色谱-串联质谱法联用监测尿液中的头孢吡肟。

Monitoring of cefepime in urine by micellar electrokinetic capillary chromatography with ultraviolet detection and liquid chromatography coupled to mass spectrometry.

机构信息

Clinical Pharmacology Laboratory, Institute for Infectious Diseases, University of Bern, Bern, Switzerland.

Department of Nephrology and Hypertension, University Hospital Bern, University of Bern, Bern, Switzerland.

出版信息

J Sep Sci. 2018 Nov;41(21):4067-4074. doi: 10.1002/jssc.201800763. Epub 2018 Sep 25.

Abstract

Cefepime monitoring in urine by micellar electrokinetic capillary chromatography with UV detection and liquid chromatography coupled to mass spectrometry via electrospray ionization is described. For micellar electrokinetic capillary chromatography, sample preparation comprised urine dilution and dodecyl-sulfate protein precipitation at pH 4.5, whereas diluted urines were analyzed in the other assay. Both approaches provided suitable conditions for cefepime analysis in urines of healthy volunteers that were spiked with cefepime. Cefepime monitoring by micellar electrokinetic capillary chromatography in samples from patients taking multiple drugs were prone to interferences, whereas liquid chromatography coupled to mass spectrometry provided clean chromatograms and thus selective detection of cefepime in all samples. The latter assay was used to measure urinary cefepime in a prospective pilot study and to assess cefepime stability in urines at 25, 4, -20 and -70°C. The data suggest that urinary cefepime is stable for at least 72 h at all tested temperatures.

摘要

本文描述了用胶束电动毛细管色谱法(MEKC)结合紫外检测和电喷雾电离液相色谱-质谱(LC-MS)联用技术对尿液中的头孢吡肟进行监测。对于 MEKC,样品制备包括尿液稀释和十二烷基硫酸钠(SDS)在 pH 4.5 时的蛋白沉淀,而在另一种方法中,对稀释的尿液进行分析。这两种方法都为健康志愿者尿液中添加头孢吡肟的头孢吡肟分析提供了合适的条件。然而,在接受多种药物治疗的患者的样本中,用 MEKC 监测头孢吡肟时容易受到干扰,而 LC-MS 则提供了干净的色谱图,从而可以选择性地检测所有样本中的头孢吡肟。后者的方法被用于前瞻性试点研究中测量尿液中的头孢吡肟,并评估在 25、4、-20 和-70°C 下尿液中头孢吡肟的稳定性。数据表明,尿液中的头孢吡肟在所有测试温度下至少稳定 72 小时。

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