首页|食用菌及其制品中过氧化麦角甾醇含量测定方法建立及应用

食用菌及其制品中过氧化麦角甾醇含量测定方法建立及应用

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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,UPLC-MS/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/z429.0/191.0;EP在5~2 000 ng·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0.020 mg·kg-1,干制食用菌制品和即食食用菌制品的EP检出限为0.040 mg·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.
Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry for Detection of Ergosterol Peroxide in Edible Fungi and Their Processed Products
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.The optimal extraction conditions were There was good linearity in the range of 5 to 2 000 ng·mL-1with 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.

Edible mushroomergosterol peroxideultra-high-performance liquid chromatography-tandem mass spectrometryquantitation

鄂恒超、彭书婷、赵志勇、张艳梅、李晓贝、周昌艳、赵晓燕

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上海市农业科学院农产品质量标准与检测技术研究所,上海 201403

食用菌 过氧化麦角甾醇 超高效液相色谱-串联质谱 含量

2024

食用菌学报
上海市农业科学院食用菌研究所,上海市农业科学院农业科技信息研究所

食用菌学报

CSTPCD北大核心
影响因子:0.771
ISSN:1005-9873
年,卷(期):2024.31(6)