Simultaneous Determination of Statins in Human Urine by Dilute-and-Shoot- Liquid Chromatography-Mass Spectrometry

• Published in: Mass spectrometry letters Vol. 9; no. 4; pp. 95 - 99
• Main Authors: Haejong Jang, Xuan-lan Mai, Gunhee Lee, Jae Hyoung Ahn, Jongsook Rhee, Quoc-ky Truong, Dinh Vinh, Jongki Hong, Kyeong Ho Kim
• Format: Journal Article
• Language: English
• Published: 한국질량분석학회 01.12.2018; 사단법인 한국질량분석학회
• Subjects: 화학; Urine; Tandem mass spectrometry; Dilute and shoot; Statins
• DOI: 10.5478/MSL.2018.9.4.95
• ISSN: 2233-4203

An innovative, simple, and rapid assay method based on liquid chromatography coupled with tandem mass spec- trometry (LC-MS/MS) was developed and validated for the simultaneous determination of eight statin drugs in human urine. A simple sample clean-up procedure using the “dilute and shoot” (DAS) approach enabled a fast and reliable analysis. The influ- ence of the dilution factor was investigated to ensure detectability and reduce the matrix effect. Chromatographic separation was performed on a Phenomenex Kinetex C18 column (50 × 3.0 mm i.d., 2.6 µm) using an elution gradient of mobile phase A com- posed of 0.1% acetic acid, and mobile phase B composed of acetonitrile, at a flow rate of 0.35 mL/min. Quantitation was per- formed on a triple quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) mode using electrospray ionization in positive ion mode. The total chromatographic run time was 15 min. The method was validated for selectivity, sen- sitivity, recovery, linearity, accuracy, precision, and stability. The present method was successfully applied to the analysis of Rosuvastatin in urine samples after oral administration to healthy human subjects. KCI Citation Count: 0