| Background:High-resolution mass spectrometry is a kind of mass spectrometry technology.It can collect accurate mass data of substances to be analyzed with wide mass range,fast scanning speed,high sensitivity,high-quality precision and high resolution.Because high-resolution mass spectrometry can screen trace components by distinguishing the impurities and co-eluting substances in complex matrices,it has great advantages in the component analysis of complex material systems.During these years,it has been widely used in controlling food safety,environmental safety and drug safety.Objective:In this paper,high-resolution mass spectrometry technology has been applyed to control the quality and safety of cosmetics and the analysis of complex unknown components.First,establishing an analytical methodology for comprehensive screening of 63 coloring agents of great concern for regulatory control in cosmetics using quadrupole-Orbitrap high-resolution mass spectrometry.Second,with the help of Q-Orbitrap high-resolution mass spectrometry,chemical constituents and plasma metabolites of precipitation and supernatant of Huang-Lian-Jie-Du-Tang have been analyzed,which provides the basis of Huang-Lian-Jie-Du-Tang precipitation becomes a new "pharmaceutical source".Research methods and result:Research object 1:coloring agents of great concern for regulatory control in cosmeticsAn analytical methodology for comprehensive screening of 63 coloring agents of great concern for regulatory control in cosmetics has been established using UHPLC-Q-Orbitrap HRMS.The cosmetic samples were pretreated by matrix solid phase dispersion(MSPD)technique,and the volume of elution solvent,the type of dispersant and elution solvent were investigated by single factor combined orthogonal test.Finally,Sand was selected as solid phase dispersant,2 mL of methanol was used for elution.By optimizing the liquid chromatography and mass spectrometry parameters,combined with the complete data processing process,the primary and secondary mass spectra can be obtained simultaneously in one injection.Quasi-deterministic analysis of compounds can be performed by alignment with accurate mass databases and secondary mass spectrometry libraries.According to method validation,63 coloring agents showed good linearity within their respective linear ranges.The in tra-day and inter-day precision,expressed as relative standard deviations(RSDs),was lower than 11%and 12%,respectively and the average recoveries varied from 64.0%to 128.4%with the RSDs between 0.9%and 10.1%,both of which meet the quantitative requirements for substances.The method is simple,accurate,rapid and sensitive,and can not only perform qualitative analysis for screening purposes,but also quantitatively detect various coloring agents in cosmetics,and is suitable for daily testing of the testing department.Research object 2:chemical composition analysis of precipitation and supernatant of Huang-Lian-Jie-Du-Tang.In the positive and negative ion mode,32 alkaloids,40 flavonoids,9 iridoids and 26 other compounds including phenolic acid and phenylpropanoid were identified.And 15 compounds were identified by comparison with retention times and MS fragmentation ions.It was found that there was no significant difference in the chemical constituents between precipitation and supernatant of Huang-Lian-Jie-Du-Tang,which provides the basis of Huang-Lian-Jie-Du-Tang precipitation becomes a new "pharmaceutical source".In addition,14 components of all detected compounds in precipitation and supernatant of Huang-Lian-Jie-Du-Tang were quantitatively investigated.A rapid and accurate UHPLC-Q-Orbitrap high-resolution mass spectrometry quantitative analysis method was established.Simultaneous quantitative detection of 14 kinds of marker substances,and comparative analysis of 14 kinds of compounds in two parts of Huang-Lian-Jie-Du-Tang.It was found that although there was no significant difference in the composition of the compound,the content of the main compound was greatly different,and the content of berberine and baicalin was greatly improved in the part of Huang-Lian-Jie-Du-Tang precipitation than in the supernatant.This experimental result provide a basis for further exploration of the mechanism of precipitation formation.Research object 3:Qualitative analysis of compounds which were absorbed into blood by gastrointestinal administration precipitation and supernatant of Huang-Lian-Jie-Du-Tang.Contrast with blank plasma,plasma sample obtained by sampling at the mixing time were detected 25 prototype ingredients,including 10 alkaloids,9 flavonoids,1 iridoid compound,and 5 other compounds including coumarin,sesquiterpene and phenylacrylic acid by UHPLC-Q-Orbitrap HRMS.Based on the theory and method of drug metabolism research,combined with the pharmacological activity of Huang-Lian-Jie-Du-Tang and other related literature reports,it is preliminarily judged that alkaloids and flavonoids may be the active ingredients of the main pharmacodynamics in Huang-Lian-Jie-Du-Tang.By comparing the compounds were absorbed into blood by gastrointestinal administration precipitation and supernatant of Huang-Lian-Jie-Du-Tang,it was found that there was no difference in the prototype components of the two parts in plasma.It can be further inferred that precipitation of Huang-Lian-Jie-Du-Tang can exert similar pharmacological effects with supernatant,and provide a basis for the pharmacological application of Huang-Lian-Jie-Du-Tang precipitation.Research conclusion:In this paper,high-resolution mass spectrometry was used to establish an analytical methodology for comprehensive screening of coloring agents in cosmetics.The method is simple,accurate,rapid,and sensitive,which can detect a variety of colorants in cosmetics The screening and identification of unknown compounds in complex Chinese medicine matrix samples and the quantitative methods of target substances were established.The differences of chemical constituents and metabolites between precipitation and supernatant of Huang-Lian-Jie-Du-Tang were compared,which provided experimental basis for the application of precipitation. |
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