Rapid detection of dihydrocodeine by thermospray mass spectrometry
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Thermospray
Thermospray
Atmospheric-pressure chemical ionization
Ambient ionization
Fragmentation
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Abstract Positive ion methane and ammonia chemical ionization mass spectra for ten phenothiazine derivatives are reported. The fragmentations observed in the chemical ionization mass spectra are rationalized in terms of the location of the added proton. High‐resolution measurements are used to confirm empirical formulae of the ions in the mass spectra. Changes in the mass spectra with a change in the chemical ionization reagent gas from methane to ammonia are described. A comparison with positive ion secondary ion mass spectra of the same compounds show that the amount of fragmentation is higher in the secondary ion mass spectra, but the same types of ions are observed in spectra produced by both ionization methods.
Fragmentation
Ambient ionization
Atmospheric-pressure chemical ionization
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Thermospray
Desorption electrospray ionization
Atmospheric-pressure laser ionization
Atmospheric-pressure chemical ionization
Ambient ionization
Field desorption
Fast atom bombardment
Capillary electrophoresis–mass spectrometry
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Thermospray
Isobutane
Fast atom bombardment
Atmospheric-pressure chemical ionization
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Abstract Chemical ionization mass spectrometry using ammonia as the reagent gas has been carried out with esters and amides of a variety of oxyacids of phosphorus (phosphates, phosphonates, phosphites and phosphoramidates). In all cases, the protonated molecular ion is a major species in the spectrum and the percentage of the total ion current carried by these protonated molecular ions is always considerably greater than that carried by the molecular ions in the corresponding electron impact mass spectra. In the chemical ionization mass spectra only limited fragmentation of the protonated molecular ion occurs from which useful information on the structure of phosphorus derivatives may be inferred.
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Polyatomic ion
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Thermospray
Atmospheric-pressure chemical ionization
Extractive electrospray ionization
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A high-performance liquid chromatograph with mass spectrum detection (HPLC-MS/APCI) method has been established for simultaneous determination of ten major bioactive components of Naodesheng injection including safflor yellow A, puerarin, daidzein, ginsenosides (Rg1, Rg2, Rb1, Rd, Re, Rh1), and notoginsenoside R1. The separations were carried out with a Luna C18 column (5 μm, 150×4.6 mm, Phenomenex, U.S.A.) with a stepwise gradient elution of the mobile phase consisting of water (0.1% of formic acid, v/v)–methanol (0 min, 70 : 30; 8 min, 30 : 70; 20 min, 10 : 90) at a flow-rate of 0.8 ml/min. The proposed method was applied to analyze five various Naodesheng injections and produced data with acceptable linearity, repeatability, precision and accuracy having lower limits of quantitation (LLOQs) of 0.02—0.2 μg. The calibration curves were linear in respective range for all compounds, all of them with coefficients of determination above 0.9900. The intraday precessions were less than 5.0%. The proposed method is accurate, sensitive and simple, a useful alternative for routine analysis in the quality control of Traditional Chinese Medicine.
Atmospheric-pressure chemical ionization
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The thermospray (TSP) mass spectra of a number of diquaternary pyridinium oxime salts, used as reactivators of organophosphate-inhibited cholinesterases, were recorded without the addition of an electrolyte. The TSP mass spectra appeared to be strongly dependent on the concentration as well as on the capillary tip temperature of the interface. At low concentrations doubly charged cations were the major fragments in most of the recorded TSP mass spectra. At concentrations well above 0.001 M as well as at too high tip temperatures more complicated spectra were obtained, probably due to fragmentation and/or decomposition. These latter spectra did correspond with the published data obtained by desorption ionization methods of these compounds. TSP mass analysis without the addition of an electrolyte appeared to be rather insensitive to the oxime salts. Using full mass scanning around 1 μg of material was necessary to produce a TSP mass spectrum.
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Fragmentation
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The characterization of several organophosphorus compounds was achieved by utilizing positive and negative ion ‘filament-on’ thermospray liquid chromatography/mass spectrometry. In the positive ion mode, the base peak was [M + NH4]+ for all the studied compounds, while in the negative ion mode the organophosphorus pesticides exhibited different fragmentation behaviour, such as electron capture, dissociative electron capture and anion attachment. The positive ion mode showed, for all the organophosphorus compounds, higher sensitivity than the negative ion mode. In the positive ion mode, detection limits at the low nanogram level were achieved for the trialkyl and triaryl phosphates, similar to gas chromatography/positive chemical ionization mass spectrometry with ammonia as reagent gas. The organophosphorus pesticides exhibited detection limits slightly lower than the phosphates, but with values similar to those previously observed in direct liquid introduction liquid chromatography/negative chemical ionization mass spectrometry. Applications of positive and negative ion analysis are reported for the determination of malathion in a fish sample.
Thermospray
Fragmentation
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