Hongyun Wang1, Pei Hu, Ji Jiang. 1. Clinical Pharmacology Research Center, Peking Union Medical College Hospital and Chinese Academy of Medical Science, Beijing, PR China. wanghongyunpumc@sohu.com
Abstract
BACKGROUND: Determination of 1-methylhistidine (1-MH) and 3-methylhistidine (3-MH) is important to monitor muscle protein catabolism. Here, an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for quantification of 1-MH and 3-MH in human urine is described. METHODS: Urine samples were prepared by dilution with water after addition of isotopic internal standard. The samples were chromatographed on a SB-aq (2.1×50 mm, 1.8 μm) column with acetonitrile -0.1% formic acid in water (2:98, v/v) as mobile phase. Mass spectrometric detection was performed on a triple quadrupole mass spectrometer using positive electrospray ionization (ESI). 1-MH and 3-MH were monitored by the following transitions: 1-MH, m/z 170.1→ m/z 126.1; 3-MH, m/z 170.1→ m/z 124.1. RESULTS: For 1-MH and 3-MH, calibration curves were linear over the concentration range of 5-500 nmol/ml. The lower limit of quantification was 5 nmol/ml. The accuracy was within 85%-115% and precision was <15%. 1-MH and 3-MH were proved to be stable under different storage and processing conditions. In addition, the detection was independent of matrix effect. CONCLUSION: This rapid and specific UPLC/MS-MS method is suitable for the determination of urinary 1-MH and 3-MH.
BACKGROUND: Determination of 1-methylhistidine (1-MH) and 3-methylhistidine (3-MH) is important to monitor muscle protein catabolism. Here, an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for quantification of 1-MH and 3-MH in human urine is described. METHODS: Urine samples were prepared by dilution with water after addition of isotopic internal standard. The samples were chromatographed on a SB-aq (2.1×50 mm, 1.8 μm) column with acetonitrile -0.1% formic acid in water (2:98, v/v) as mobile phase. Mass spectrometric detection was performed on a triple quadrupole mass spectrometer using positive electrospray ionization (ESI). 1-MH and 3-MH were monitored by the following transitions: 1-MH, m/z 170.1→ m/z 126.1; 3-MH, m/z 170.1→ m/z 124.1. RESULTS: For 1-MH and 3-MH, calibration curves were linear over the concentration range of 5-500 nmol/ml. The lower limit of quantification was 5 nmol/ml. The accuracy was within 85%-115% and precision was <15%. 1-MH and 3-MH were proved to be stable under different storage and processing conditions. In addition, the detection was independent of matrix effect. CONCLUSION: This rapid and specific UPLC/MS-MS method is suitable for the determination of urinary 1-MH and 3-MH.
Authors: Yuko Yamaguchi; Marta Zampino; Ruin Moaddel; Teresa K Chen; Qu Tian; Luigi Ferrucci; Richard D Semba Journal: Metabolomics Date: 2021-01-11 Impact factor: 4.747
Authors: Gabriela de Matuoka E Chiocchetti; Leisa Lopes-Aguiar; Natália Angelo da Silva Miyaguti; Lais Rosa Viana; Carla de Moraes Salgado; Ophelie Ocean Orvoën; Derly Florindo; Rogério Williams Dos Santos; Maria Cristina Cintra Gomes-Marcondes Journal: Metabolites Date: 2021-06-20