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  • P-ISSN2233-4203
  • E-ISSN2093-8950
Search Word: experimental design, Search Result: 1
1
Thuy-Vy Pham(Kangwon National University) ; Gunhee Lee(Kangwon National University) ; Xuan-Lan Mai(Ho Chi Minh City University of Technology (HUTECH)) ; Thi-Anh-Tuyet Le(Kangwon National University) ; Thi Ngoc Van Nguyen(Can Tho University of Medicine and Pharmacy) ; Jongki Hong(Kyung Hee University) ; Kyeong Ho Kim(Kangwon National University) 2021, Vol.12, No.1, pp.1-10 https://doi.org/10.5478/MSL.2021.12.1.1
초록보기
Abstract

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.

Mass Spectrometry Letters