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  • P-ISSN 2233-4203
  • E-ISSN 2093-8950

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

Mass Spectrometry Letters / Mass Spectrometry Letters, (P)2233-4203; (E)2093-8950
2018, v.9 no.4, pp.95-99
https://doi.org/10.5478/MSL.2018.9.4.95
Haejong Jang (Kangwon National University)
Xuan Lan Mai (Kangwon National University)
Gunhee Lee (Kangwon National University)
Jae Hyoung Ahn (Kangwon National University)
Jongsook Rhee (National Forensic Service Busan Institute)
Quoc-Ky Truong (Pham Ngoc Thach University of Medicine)
Dinh Vinh (University of Medicine and Pharmacy Ho Chi Minh City)
Jongki Hong (Kyung Hee University)
Kyeong Ho Kim (Kangwon National University)
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Abstract

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.

keywords
Statins, Urine, Dilute and shoot, Tandem mass spectrometry


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투고일Submission Date
2018-10-01
수정일Revised Date
2018-11-16
게재확정일Accepted Date
2018-11-19
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