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

A Dilute-and-Shoot LC–MS/MS Method for Screening of 43 Cardiovascular Drugs in Human Urine

Mass Spectrometry Letters / Mass Spectrometry Letters, (P)2233-4203; (E)2093-8950
2021, v.12 no.1, pp.1-10
Pham Thuy-Vy (Kangwon National University)
Lee Gunhee (Kangwon National University)
Mai Xuan-Lan (Ho Chi Minh City University of Technology (HUTECH))
Le Thi-Anh-Tuyet (Kangwon National University)
Nguyen Thi Ngoc Van (Can Tho University of Medicine and Pharmacy)
Hong Jongki (Kyung Hee University)
Kim Kyeong Ho (Kangwon National University)
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A simple, specific, and economical LC–MS/MS method was investigated for the screening of 43 prescribed antihy-pertensive and related drugs in human urine. The urine samples were simply prepared by diluting and mixing with internal stan-dard before directly introduced to the LC-MS/MS system, which is fast, straightforward, and cost-effective. Fractional factorial, Box-Behnken, and I-optimal design were applied to screen and optimize the mass spectrometric and chromatographic factors. The analysis was carried out on a triple quadrupole mass spectrometer system utilizing multiple reaction monitoring with posi-tive and negative electrospray ionization method. Chromatographic separation was performed on a Thermo Scientific Accucore RP-MS column (50 × 3.0 mm ID., 2.6 µm) using two separate gradient elution programs established with the same mobile phases. Chromatographic separation was performed within 12 min. The optimal method was validated based on FDA guideline. The results indicated that the assay was specific, reproducible, and sensitive with the limit of detection from 0.1 to 50.0 µg/L. The method was linear for all analytes with coefficient of determination ranging from 0.9870 to 0.9981. The intra-assay preci-sion was from 1.44 to 19.87% and the inter-assay precision was between 2.69 and 18.54% with the recovery rate ranges from 84.54 to 119.78% for all drugs measured. All analytes in urine samples were stable for 24 h at 25 o C, and for 2 weeks at -60 o C. The developed method improves on currently existing methods by including larger number of cardiovascular medications and better sensitivity of 12 analytes.

antihypertensive drugs, screening test, dilute-and-shoot LC-MS/MS, experimental design

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Mass Spectrometry Letters