| Phthalate esters(PAEs)can improve the flexibility,durability,and ductility of plastic products,so they are added to plastic products in large quantities as plasticizers.Phthalates are a kind of common environmental estrogens,which can cause endocrine disorders in the human body,stimulate potential cancer cells and mutagenicity,and have serious harm to human health.Phthalates are easily migrated from plastics to food contact,posing certain food safety risks.Edible and medicinal fungi are widely welcomed by consumers because of their nutritional value and health care effects.Triterpenes and sterols are the main chemical components,which have anti-tumor and anti-inflammatory effects,and are one of the important indicators for the quality evaluation of edible and medicinal fungi.The safety of edible and medicinal fungi products has also attracted much attention,and the content of phthalates has also been concerned recently.Therefore,in this paper(1)a new method for the detection of phthalates in edible and medicinal fungi was proposed to be established;(2)an improved ultraviolet-visible spectrophotometric method for triterpenes and sterols;(3)Collect fungi samples for verification.The review part introduces the research status of phthalates,triterpenes,and sterols and their detection methods at home and abroad.The research content is divided into three chapters.Including the establishment of a method for the detection of 23 kinds of phthalates in edible and medicinal fungi by ultra-high performance liquid phase-tandem mass spectrometry(UPLC-MS/MS);The 14 kinds of edible and medicinal fungi purchased were detected and analyzed for phthalates;the content of triterpenes and sterols in 36 kinds of fungi was detected by optimized and improved ultraviolet-visible spectrophotometry.In the first chapter of the research part,the key factors that affect the peak shape and the response value of each target,such as different mobile phases,column temperatures,chromatographic columns,and ultrafiltration membranes,are optimized,and the blank interference to the liquid phase system by adding trapping columns to exclude,use the Intellistart tuning program of UPLC-MS/MS to select the optimal mass spectrometry detection conditions for each target substance.The results showed that the mobile phase was methanol-water,the column temperature was 35℃,the phenyl column CSHTM Phenyl-Hexyl was selected,the PTFE ultrafiltration membrane was selected,and the trapping column Ghost-Buster HP Column was added,and Diisononyl ortho-phthalate(DINP),Dinonyl phthalate(DNP),Dibutyl phthalate(DBP),Diisobutyl phthalate(DIBP),Bis(2-ethylhexyl)phthalate(DEHP),Di-n-octyl phthalate(DNOP),Di-n-pentyl phthalate(DPP),Diisopentyl phthalate(DIPP),Didecyl phthalate(DNDP),Diethyl phthalate ester(DEP),Dicyclohexyl phthalate(DCHP),Dipropyl phthalate(DPrP),Diisopropyl phthalate(DIPrP),Diphenyl phthalate(DPhP),Di-n-hexyl phthalate(DNHP),Bis(2-methoxyethyl)phthalate(DMEP),Diallyl phthalate(DAP),Benzyl butyl phthalate(BBP),Dimethyl phthalate(DMP),N-octyl-n-decyl phthalate(ODP),Diisooctyl phthalate(DIOP),Diisodecyl ortho-phthalate(DIDP),and Dibenzyl phthalate(DBzP).The detection conditions of a total of 23 phthalates were optimal.Combined with the tuning program,the cone voltage and collision energy were optimized,and the product ion fragments with relatively high relative abundance and stable peaks were selected.Finally,a rapid and accurate UPLC-MS/MS method for the detection of 23 phthalates in edible and medicinal fungi.The 23 phthalates have a good linear relationship within a certain concentration range,the correlation coefficient R2 is all greater than 0.9952,the sample recovery rate is 79.4%～104.3%,the RSD is 4.3%～10.7%,the limit of quantification(S/N≥ 10)0.2μg/kg～8.0μg/kg is lower than the national standard limit,which provides a new technical means for the detection of phthalate content in edible and medicinal fungi.In the second chapter of the research part,14 kinds of edible and medicinal fungi purchased from the market were tested for phthalate content.The results showed that 14 edible and medicinal fungi Sarcomyxa edulis,Lentinula edodes,Pleurotus citrinopileatus,Pholiota nameko,Lyophyllum decastes,Tremella fuciformis,and Auricularia heimuer all detected Dibutyl phthalate DBP and Diisobutyl phthalate DIBP,and the DBP content both exceeded the national standard limit of 0.3 mg·kg-1,among which Auricularia heimuer and Tremella fuciformis also detected that the Diethyl phthalate DEP was 0.05 mg·kg-1 and 0.02 mg·kg-1.In the third chapter of the research part,the detection method of triterpenes and sterols in the medicinal fungi Ganoderma lucidum in the 2020 edition of the Pharmacopoeia of the People’s Republic of China was optimized,the content of triterpenoids and sterols in 36 kinds of fungi samples were determined by the improved method.The results show that the maximum absorption wavelength of oleanolic acid is 555 nm after wavelength scanning,which is higher than 546 nm in the 2020 edition of the Pharmacopoeia of the People’s Republic of China.Within a certain concentration range,the linear relationship is good,and the correlation coefficient R2 is 0.9995.The repeatability was good,the average recovery rate of sample addition was 99.24%,and the RSD was 1.28%,which verified the feasibility of using the improved ultraviolet-visible spectrophotometry to detect the content of triterpenes and sterols in fungi.The triterpenes and sterol contents of Inonotus hispidus and Sparassis crispa in the polypore were 3.36%and 3.27%,which were significantly higher than those of other groups.Among the three myxomycetes,Stemonitis splendens,Ceratiomyxa fruticulosa,and Fuligo septica also detected triterpenes and sterols content of 1.01%,1.05%,and 0.77%,respectively.In summary,this paper established an ultra-high performance liquid phase-tandem mass spectrometry(UPLC-MS/MS)method for the detection of 23 phthalates in edible and medicinal fungi,and analyzed 14 commercially available edible and medicinal fungi have been verified by the method,which will provide important support for the formulation of quality and safety supervision standards for edible and medicinal fungi products in the future;the content of triterpenes and sterols in 36 species of fungi was determined by optimized ultraviolet-visible spectrophotometry,which is accurate Determination of triterpenes and sterols in fungi provides data reference and theoretical basis. |
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