Mass Spectrometry Letters

Korean Society for Mass Spectrometry (한국질량분석학회)
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Simultaneous Determination of Statins in Human Urine by Dilute-and-Shoot-Liquid Chromatography-Mass Spectrometry

  • Jang, Haejong (College of Pharmacy, Kangwon National University) ;
  • Mai, Xuan-Lan (College of Pharmacy, Kangwon National University) ;
  • Lee, Gunhee (College of Pharmacy, Kangwon National University) ;
  • Ahn, Jae Hyoung (College of Pharmacy, Kangwon National University) ;
  • Rhee, Jongsook (Forensic Toxicology & Chemistry Division, National Forensic Service Busan Institute) ;
  • Truong, Quoc-Ky (Faculty of Pharmacy, Pham Ngoc Thach University of Medicine) ;
  • Vinh, Dinh (University of Medicine and Pharmacy Ho Chi Minh City) ;
  • Hong, Jongki (College of Pharmacy, Kyung Hee University) ;
  • Kim, Kyeong Ho (College of Pharmacy, Kangwon National University)
  • Received : 2018.10.01
  • Accepted : 2018.11.19
  • Published : 2018.12.30
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Abstract

An innovative, simple, and rapid assay method based on liquid chromatography coupled with tandem mass spectrometry (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 influence of the dilution factor was investigated to ensure detectability and reduce the matrix effect. Chromatographic separation was performed on a Phenomenex Kinetex C18 column ($50{\times}3.0mm$ i.d., $2.6{\mu}m$) using an elution gradient of mobile phase A composed of 0.1% acetic acid, and mobile phase B composed of acetonitrile, at a flow rate of 0.35 mL/min. Quantitation was performed 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, sensitivity, 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

E1MPSV_2018_v9n4_95_f0001.png 이미지

Figure 1. Chemical structures of eight statin drugs and internal standard (IS)

E1MPSV_2018_v9n4_95_f0002.png 이미지

Figure 2. Total chromatogram of eight statins and internal standard. (1) Pravastatin (2) Pitavastatin (3) Rosuvastatin D6 (4) Rosuvastatin (5) Fluvastatin (6) Atorvastatin (7) Mevastatin (8) Lovastatin (9) Simvastatin

E1MPSV_2018_v9n4_95_f0003.png 이미지

Figure 3. Accumulative excretion of rosuvastatin in urine

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