首页|超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速检测菌类中鹅膏毒肽毒素

超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速检测菌类中鹅膏毒肽毒素

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采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定蘑菇中3种鹅膏肽类毒素的含量[α-鹅膏毒肽(α-AMA)、β-鹅膏毒肽(β-AMA)和γ-鹅膏毒肽(γ-AMA)].将样品均质后,利用甲酸-甲醇-水(0.5∶10∶89.5,v/v/v)标准混合溶液提取,经由BEH shield RP18柱(150 mm × 2.1 mm,1.7 μm)实施分离,采取梯度洗脱,流动相为0.03%氨水与甲醇,在HESI离子化方式下以tSIM正离子模式进行扫描检测,外标法定量.蘑菇所含3类鹅膏肽类毒素具良好线性关系,区间是0.05 mg/kg~5 mg/kg,相关系数r均在0.995以上,确定α-AMA、γ-AMA检出限是0.01 mg/kg,定量限是0.02 mg/kg;β-AMA的检出限和定量限分别为0.02 mg/kg和0.05 mg/kg.平均回收率于3个加标水平下处在72.5%~91.9%范围,相对标准偏差(RSD,n=6)为2.8%~7.4%.方法简单高效,适用于蘑菇中3种鹅膏肽类毒素(α-AMA、β-AMA和γ-AMA)的快速检测.
Rapid Determination of Amanita Peptide Toxins in Mushrooms by Ultra Performance Liquid Chromatography-Q Exactive orbitrap high-resolution mass spectrometry
The ultra performance liquid chromatography-Q Exactive orbitrap high-resolution mass spectrometry method was established for the rapid determination of 3 kinds of amanita peptide toxins in mushrooms.The sample was abstracted with the standard mixed solution of formic acid-methanol-water(0.5∶10∶89.5,v/v/v)after ho-mogenized.The amanita peptide toxins were purified with BEH shield RP18 chromatographic analysis column elu-tion(150 mm ×2.1 mm,1.7 μm),Gradient elution with a mobile phase of 0.03%ammonia.tSIM positive ion mode scanning was used for detection under HESI,and quantitative analysis was carried out by external standard method.The linearities of 3 kinds of amanita peptide toxins in mushrooms were good in range of 0.05 ng/mL to 5 mg/kg,correlation coefficients r were all above 0.995,and the detection limit of α-amanitracin(α-AMA)and α-amanitracin(γ-AMA)was 0.01 mg/kg,and the limit of quantitation was 0.02 mg/kg.The values of β-AMA were 0.02 mg/kg and 0.05 mg/kg respectively.The average recovery was in the range of 72.5%~91.9%at the three added levels,and the relative standard deviation(RSD,n=6)was 2.8%~7.4%.This method is simple and efficient.It can be applied to rapid detection of 3 kinds of amanita peptide toxins in mushrooms.

amanitinsmushroomsUltra Performance Liquid Chromatography-Q Exactive orbitrap high-resolu-tion mass spectrometry

蒋云露、吴文林、黄弋耘、夏鸿玲、吴丹、郭添荣、孙群、张敏

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成都市食品检验研究院 611130

中国科学院成都生物研究所 610041

中国科学院大学 100049

成都理工大学地质灾害防治与地质环境保护国家重点实验室 610059

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鹅膏毒肽 蘑菇 超高效液相色谱-四极杆/静电场轨道阱高分辨质谱

科技部国家重点研发专项四川省重点研发项目

2022YFF07104052022YFS0511

2024

粮食储藏
国家粮食储备局成都粮科所 中国粮油学会储藏专业分会

粮食储藏

影响因子:0.589
ISSN:1000-6958
年,卷(期):2024.53(4)