| Literature DB >> 24521423 |
Linfan Li1, Tsung-Chi Chen, Yue Ren, Paul I Hendricks, R Graham Cooks, Zheng Ouyang.
Abstract
A benchtop miniature mass spectrometer system, Mini 12, with ambient ionization source and tandem mass spectrometry capabilities has been developed and characterized. This instrument was developed as a self-contained system to produce quantitative results for unprocessed samples of small volumes including nonvolatile analytes. The ion processing system, vacuum system, and control system are detailed. An integrated sample loading system facilitates automated operation. A user interface has been developed to acquire and to interpret analytical results for personnel who have limited mass spectrometry knowledge. Peak widths of Δm/z 0.6 Th (full width at half-maximum) and a mass range of up to m/z 900 are demonstrated with the rectilinear ion trap mass analyzer. Multistage experiments up to MS(5) are accomplished. Consumable cartridges have been designed for use in ambient paper spray ionization, and the recently developed extraction spray ionization method has been employed to improve the quantitative performance. Monitoring of trace-levels of chemicals in therapeutic drugs, as well as in food safety and environmental protection operations is demonstrated. Dual MS/MS scans are implemented to obtain the intensities of the fragment ions from the analyte and its internal standard, and the ratio is used in quantitative analysis of complex samples. Limits of quantitation (LOQ) of 7.5 ng/mL, with relative standard deviations below 10%, have been obtained for selected therapeutic drugs in whole blood throughout their individual therapeutic ranges.Entities:
Mesh:
Year: 2014 PMID: 24521423 PMCID: PMC3985695 DOI: 10.1021/ac403766c
Source DB: PubMed Journal: Anal Chem ISSN: 0003-2700 Impact factor: 6.986
Figure 1(a) Mini 12 system that provides a simplified operational protocol. (b) Flowchart for automated quantitative analysis using an internal standard. (c) Operation of the dual MS/MS scan function in the time domain.
Figure 2(a) Overview of Mini 12 system and (b) selected subsystems showing ion generation, introduction, and analysis. (c) Design of paper spray sample cartridge used with the Mini 12 system. (d) Schematic diagram of the control electronics in the Mini 12 system.
Figure 3(a) Mass spectrum of 1 ppm clenbuterol recorded using nanoESI with RIT operated at rf frequency 1000 kHz with resonance ejection at 350 kHz (q = 0.80) and ac amplitude ramped from 1.5 to 3.0 Vp–p. (b) Mass spectrum of 5 ppm tacrolimus, 1 ppm imatinib, and 1 ppm amitriptyline mixture recorded using nanoESI and RIT rf frequency 1000 kHz and resonance ejection at 300 kHz and 3.5–7.5 Vp–p. (c) Mass spectrum of MS2 of 500 ppt thiabendazole in 50/50 MeOH/H2O using nanoESI. (d) Mass spectrum of MS5 of 20 ppm clenbuterol in 50/50 MeOH/H2O using nanoESI (inset shows the isolated peak of ions with m/z 168).
Figure 4MS/MS spectra of (a) 50 ng of amitriptyline in blood recorded with paper spray ionization and (b) extraction spray ionization. MS/MS spectra of (c) thiabendazole on an orange peel obtained using paper spray ionization.
Figure 5Ion intensity of 200 ng/mL amitriptyline and 100 ng/mL amitriptyline-d6 (IS) in blood with (a) paper spray ionization with silica-coated paper and (b) extraction spray ionization. (c) Ratio of amitriptyline/amitriptyline-d6 in adjacent MS/MS scans using extraction spray ionization and paper spray ionization. (d) Calibration curve showing ratio of amitriptyline/amitriptyline-d6 in blood with extraction spray ionization (product ion m/z of 233 was monitored).