Abstract
A ultrahigh performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF/MS) method was developed for simultaneous determination of 8 endogenous alkaloid compounds inBoletus.Boletussamples were extracted by 50% (V/V) methanol-water solution, then separated by CORTECS UPLC HILIC column using a binary solvent system by gradient elution. The analytes were determined by Q-TOF/MS in TOF MS and information dependent acquisition (IDA)-MS/MS mode. The results showed that mass accuracy error of the 8 endogenous alkaloids were lower than 5.0 × 10−6, good linear relationship was got in range of 0.2–500 μg/L, and correlation coefficient was higher than 0.9990. The limit of detection was in the range of 0.002–0.100 mg/kg and the limit of quantification was in the range of 0.004–0.200 mg/kg. Recovery of the method was in range of 80.1%–101.5% with spike levels of 0.004–2.00 mg/kg, relative standard deviations were lower than 10%. The method was simple, specific, and reliable. It could be used for the rapid screening and quantitative analysis of 8 endogenous alkaloids inBoletus.
Highlights
Materials and MethodsEvery five samples were run, and the mass accuracy calibration was automatically performed
Introduction eBoletus is an edible fungus belonging to the Fungi, Basidiomycotina, Hymenomycetes, Agaricates [1]
Validation of the whole analytical method was performed with linearity, the limit of detection (LOD), the limit of quantification (LOQ), precision, accuracy, and recovery. e linearity of the method was evaluated by constructing calibration curves with different concentrations of 8 alkaloids. e LOD and LOQ under the present chromatographic conditions were calculated on the basis of the response and slope of each regression equation at signalto-noise ratios (S/N) of 3 : 1 and 10 : 1, respectively. e recoveries of analytes were evaluated by adding the standard solutions with three different concentration levels (1x LOQ, 3x LOQ, 10x LOQ) to the known amounts of fungus samples, and each level was repeated six times. e precision of the method was expressed by a relative standard deviation (RSD)
Summary
Every five samples were run, and the mass accuracy calibration was automatically performed. E experiment investigated the response of target compounds under positive and negative ionization modes. Validation of the whole analytical method was performed with linearity, the limit of detection (LOD), the limit of quantification (LOQ), precision, accuracy, and recovery. E recoveries of analytes were evaluated by adding the standard solutions with three different concentration levels (1x LOQ, 3x LOQ, 10x LOQ) to the known amounts of fungus samples, and each level was repeated six times.
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