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1.
Journal of Pharmaceutical Analysis ; (6): 293-300, 2022.
Article in Chinese | WPRIM | ID: wpr-931257

ABSTRACT

A rapid and sensitive method for analyzing trace β-blockers in complex biological samples,which involved magnetic solid-phase extraction(MSPE)coupled with Fourier transform ion cyclotron reso-nance mass spectrometry(FTICR-MS),was developed.Novel nanosilver-functionalized magnetic nano-particles with an interlayer of poly(3,4-dihydroxyphenylalanine)(polyDOPA@Ag-MNPs)were synthesized and used as MSPE adsorbents to extract trace β-blockers from biological samples.After extraction,the analytes loaded on the polyDOPA@Ag-MNPs were desorbed using an organic solvent and analyzed by FTICR-MS.The method was rapid and sensitive,with a total detection procedure of less than 10 min as well as limits of detection and quantification in the ranges of 3.5-6.8 pg/mL and 11.7-22.8 pg/mL,respectively.The accuracy of the method was also desirable,with recoveries ranging from 80.9%to 91.0%following the detection of analytes in human blood samples.All the experimental results demonstrated that the developed MSPE-FTICR-MS method was suitable for the rapid and sensitive analysis of trace β-blockers in complex biological samples.

2.
Chinese Journal of Analytical Chemistry ; (12): 1125-1131, 2014.
Article in Chinese | WPRIM | ID: wpr-454911

ABSTRACT

A new method for the determination of organic acids from mainstream cigarette smoke using ultra low temperature solvent extraction-comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry(GC×GC-TOF/MS)was established. The mainstream smoke was directly trapped by ethyl ether with ultra low temperature solvent extraction device, and cleaned up with liquid-liquid extraction. The concentrated extracts were further derived by N,O-bis(trimethylsily)trifluoroacetamide (BSTFA). The good separation of silanized product was achieved by the column set of DB-1 (30 m × 0. 25 mm, 1. 0 μm) as the 1st column and DB-wax (1. 5 m × 0. 1 mm, 0. 1 μm) as the 2nd column with modulation period of 6 s and scan range of m/z 45-450 . The results showed that linearity correlation coefficients were larger than 0 . 99 , and the average recoveries were between 80. 17% and 107. 81% with the relative standard deviations (RSD) in the range of 0 . 4%-12 . 1% ( n=5 ) . The detection limit and the quantitation limit were 1 . 3-24 . 5 μg/kg and 4. 1-77. 1 μg/kg, respectively.

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