摘要
为建立食用菌及其制品中过氧化麦角甾醇(ergosterol peroxide,EP)含量的测定方法,采用超高效液相色谱-串联质谱(ultra-high-performance liquid chromatography-tandem mass spectrometry,UPLCMS/MS)法优化色谱、质谱条件,通过基质效应、加标回收率、检出限和重复性实验考察方法学,最后采用建立的方法测定31种食用菌及其制品中的EP含量。结果表明:采用C18色谱柱,流动相为0.1%甲酸甲醇∶0.1%甲酸水=92∶8(V∶V),采用乙腈为提取溶剂30℃超声提取30 min,定量离子选用m/z 429.0/191.0;E P在5~2000n g·mL^(-1)内线性关系良好,基质效应较弱;鲜品和腌制食用菌制品的EP检出限为0.020m g·kg^(-1),干制食用菌制品和即食食用菌制品的EP检出限为0.040mg·kg^(-1);加标回收率为78.4%~111.5%,符合GB 2763—2021中60%~120%的要求;日内变异系数和日间变异系数分别为0.3%~4.8%和0.4%~2.0%;在鲜品中香菇的EP含量较高。
Using ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),a method was established for measuring ergosterol peroxide(EP)content in edible fungi and their processed products through optimizing chromatographic conditions,mass spectrometric parameters,extraction solvents,extraction time,and temperature.The method was validated through matrix effect assessment,spike-and-recovery testing,and evaluation of repeatability and reproducibility.The established method was used to measure EP content in 31 samples of edible fungi and processed products.The results showed that the chromatographic conditions were using a C18 chromatographic column and isocratic elution with 0.1%formic acid in methanol and 0.1%formic acid in water at a volumetric ratio of 92:8.Aacetonitrile was used as the extraction solvent for ultrasonic extraction at 30℃for 30 min.The quantitative ion transition was m/z 429.0/191.0.-1 The optimal extraction conditions were There was good linearity in the range of 5 to 2000 ng·mL with minimal matrix effects.The EP detection limit for fresh and pickled edible fungi products was 0.020 mg·kg^(-1),and that of dried and ready-to-eat edible fungi products was 0.040 mg·kg^(-1).The spike recovery rates were 78.4%–111.5%,which comply with the national standard of 60%–120%in GB 2763-2021.The intraday variation coefficients and interday variation coefficients were 0.3%–4.8%,and 0.4%–2.0%,respectively.Fresh L.edodes had a relatively high EP content.
作者
鄂恒超
彭书婷
赵志勇
张艳梅
李晓贝
周昌艳
赵晓燕
E Hengchao;PENG Shuting;ZHAO Zhiyong;ZHANG Yanmei;LI Xiaobei;ZHOU Changyan;ZHAO Xiaoyan(Institute of Agri-food Standards and Testing Technology,Shanghai Academy of Agricultural Sciences,Shanghai 201403,China)
出处
《食用菌学报》
CSCD
北大核心
2024年第6期112-118,共7页
Acta Edulis Fungi
基金
国家重点研发计划青年科学家项目(2023YFD1601000)
上海市农业科学院2024年度农业科技创新支撑领域研究专项[农科应基2024(09)]。
关键词
食用菌
过氧化麦角甾醇
超高效液相色谱-串联质谱
含量
Edible mushroom
ergosterol peroxide
ultra-high-performance liquid chromatography-tandem mass spectrometry
quantitation
