[Determination of beta2-agonists and beta-blockers in urine using high performance liquid chromatography-ion trap mass spectrometry].
A method has been developed for the determination of 23 beta2-agonists and 5 beta-blockers in urine samples using high performance liquid chromatography-ion trap mass spectrometry (HPLC-IT-MS). Urine samples were first deproteinized by high-speed frozen centrifugation, and the supernatants were loaded on an Extrelut diatomite column for clean-up. The analytes were eluted by ethyl acetate and concentrated for further analysis. The analytical separation was performed on an AtlantisT3-150 mm chromatographic column with the gradient elution using methanol and water (containing 0.1% formic acid). The detection was carried on a linear ion trap mass spectrometer under multiple reaction monitoring (MRM) mode with the source operated in positive mode of electrospray ionization (ESI+). Nine deuterium labeled beta2-agonists were used as internal standards for quantitative analysis. The results showed that the linear ranges for 23 beta2-agonists and 5 beta-blockers were 0.005-0.16 mg/L, and the limits of detection were all around 0.2 microg/L. The mixed standard solution was added into the blank urine samples, and the recoveries of 23 beta2-agonists and 5 beta-blockers were ranged from 57.1% to 127.7% with the relative standard deviations of 1.1%-31.1%. The results demonstrate that the method is easy, fast, sensitive, and suitable for the confirmation and quantification of 23 beta2-agonists and 5 beta-blockers in urine samples.
Miao
Hong
H
Institute of Nutrition and Food Safety, Chinese Centre for Disease Control and Prevention, Beijing 100021, China.
Zou
Jianhong
J
Fan
Sai
S
Gan
Lewen
L
Zhao
Yunfeng
Y
Wu
Yongning
Y
D058666:Adrenergic beta-2 Receptor Agonists / Q000652:urine*; D000319:Adrenergic beta-Antagonists / Q000652:urine*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006801:Humans; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
D058666:Adrenergic beta-2 Receptor Agonists; D000319:Adrenergic beta-Antagonists