Abstract
Rapid qualitative and quantitative analysis of solid samples (e.g., pharmaceutical preparations) by using a small and low-resolution mass spectrometer without MS/MS function is still a challenge in ambient pressure ionization mass spectrometric analysis. Herein, a practically efficient method termed microwave-enhanced in-source decay (MEISD) using microwave plasma torch desorption ionization coupled with time-of-flight mass spectrometry (MPTDI-TOF MS) was developed for fast analysis of pharmaceutical tablets using a miniature TOF mass spectrometer without tandem mass function. The intensity of ISD fragmentation was evaluated under different microwave power values. Several factors, including desorption distance and time that might affect the signal intensity and fragmentation, were systematically investigated. It was observed that both the protonated molecular ions and major fragment ions from the active ingredients in tablets could be found in the full-scan mass spectra in positive ion mode, which were comparable to those obtained by a commercial LTQ-XL ion trap mass spectrometer. The structures of the ingredients could be elucidated in detail using the MEISD method, which promotes our understanding of the desorption/ionization processes in microwave plasma torch (MPT). Quantitative analysis of 10 tablets was achieved by full-scan MPTDI-TOF MS with low limit of detection (LOD, 0.763 mg/g), acceptable relative standard deviation (RSD < 7.33%, n =10), and 10 s for each tablet, showing promising applications in high throughput screening of counterfeit drugs.Graphical ᅟ
Highlights
Identification and authentication of pharmaceuticals can be confidently achieved by mass spectrometry, which provides plentiful molecular information to probe the chemical nativityR
Since the matrix is not removed in ambient mass spectrometry, multiple stage mass spectrometry experiments are normally required to obtain characteristic fragments of each analyte to exclude any potential false positive signals
Analysis was conducted with a time-of-flight mass spectrometer (TOF-MS 5000; Hexin Mass Spectrometry, Guangzhou, China) equipped with a microwave plasma torch (MPT) source with standard voltage, pressure, distance, and angling capability (Changchun Jilin University Little Swan Instrument, Jilin, China)
Summary
Identification and authentication of pharmaceuticals can be confidently achieved by mass spectrometry, which provides plentiful molecular information to probe the chemical nativityR. Identification and authentication of pharmaceuticals can be confidently achieved by mass spectrometry, which provides plentiful molecular information to probe the chemical nativity. Since the matrix is not removed in ambient mass spectrometry, multiple stage mass spectrometry experiments are normally required to obtain characteristic fragments of each analyte to exclude any potential false positive signals. Either a mass spectrometry instrument with extremely high resolution for exact mass measurement [15, 16] or tandem mass spectrometry capability (MSn, n ≥ 2) [17] is required to obtain confident results. At present, advanced instruments required to achieve either high mass resolution or multiple stage mass spectrometry experiments impose high cost, large size, and heavy weight on the mass spectrometers
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