Wuzi-Yanzong-Wan (WZYZW), a classical traditional Chinese medicine (TCM) prescription containing Fructus Lych, Semen Cuscutae (fried), Fructus Rubi, Fructus Schisandrae chinensis (steamed) and Semen Plantaginis (fried with salt), is widely used to treat impotence, sterility, spermatorrhea, premature ejaculation, lumbago and post-micturation dribble. However, the chemical profile of WZYZW has not been established yet. In this work, a rapid and sensitive method for systematically screening and identifying the chemical constituents of WZYZW in both positive and negative ion modes using Ultra-Performance LC coupled with ESI-linear ion trap-Orbitrap tandem mass spectrometry (UPLC-ESI-LTQ-Orbitrap-MS) has been developed. Based on the chromatographic and spectrometric data, and referring to the literature, we could tentatively identify 106 compounds, including organic acids, flavonoids, phenylpropanoids, alkaloids and terpenoids. Fourteen ingredients from Fructus Lych were identified, while 10 ingredients were from Semen Cuscutae (fried), 33 ingredients were from Fructus Rubi, 37 ingredients were from Fructus Schisandrae chinensis (steamed), and 20 ingredients were from Semen Plantaginis (fried with salt). The results may provide essential data for further quality control, pharmacological research and clinical evaluation of WZYZW. Furthermore, this study indicates the developed approach based on UPLC-ESI-LTQ-Orbitrap-MS is suitable for characterizing the chemical profiles of TCM prescriptions. This is the first report to provide a comprehensive analysis of the chemical constituents of WZYZW.
The aim of this study is to develop and validate an improved analytical method for the simultaneous quantification of 20 types of mycotoxins in grapes and wines. In this research, the optimization of tandem mass spectrometer (MS/MS) parameter, ultra-high pressure liquid chromatography (UHPLC) separation, and QuEChERS procedure, which includes wine/water ratio, the amount and type of salt, clean-up sorbent, were performed, and the whole separation of mycotoxins was accomplished within 7 min analyzing time. Under optimum conditions, recoveries ranged from 85.6% to 117.8%, while relative standard deviation (RSD) remained between 6.0% and 17.5%. The limit of detection (LOD, 0.06–10 μg/L) and the limit of quantification (LOQ, 0.18–30 μg/L) were lower than those permitted by legislation in food matrices, which demonstrated the high sensitivity and applicability of this efficient method. Finally, 36 grapes and 42 wine samples from the Hexi Corridor region were analyzed. Penicillic acid (PCA), mycophenolic acid (MPA), cyclopiazonic acid (CPA), fumonisin B1 (FB1) and zearalenone (ZEN) were detected in a small number of grape samples with lower concentrations between 0.10 μg/L and 81.26 μg/L. Meanwhile, ochratoxin A (OTA), aflatoxin B2 (AFB2), MPA, CPA, and ZEN were detected in some wine counterparts with concentrations ranged from 0.10 μg/L to 4.62 μg/L. However, the concentrations of the detected mycotoxins were much lower than the maximum legal limits set of other products.
To investigate the pyrolysis characteristics of waste tire, an analytical pyrolyzer coupled with gas chromatography/ mass spectrometry (Py−GC/MS) setup had been proposed. Waste tire was pyrolyzed under different temperatures. Results showed that the primary pyrolysis products of waste tire at 600°C were alkenes rather than alkanes or aromatics. Isoprene (18.7%) and D-limonene (22.9%) represented the main compounds of chain alkenes and cyclic alkenes, respectively. The degradation procedure of D-limonene was also investigated. It could be indicated that, when the temperature was 500°C and below, isomerized alkenes of D-limonene were the main products. With the temperature increasing to 600°C and above, aromatics began to raise. According to the product distribution, eight pyrolysis reaction pathways of D-limonene were proposed. Pyrolysis of waste tire under different temperatures proved that the reaction pathways of D-limonene were reliable. Moreover, a thermogravimetric analyzer coupled with Fourier transform infrared spectroscopy (TG-FTIR) investigation also consolidated the main processes proposed by Py−GC/MS. These findings provide some references for the pyrolysis mechanism of waste tires.
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