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采用高效液相色谱-电喷雾电离质谱法测定镰刀菌霉菌毒素、镰刀菌增殖素和白僵菌素。

Determination of the Fusarium mycotoxins, fusaproliferin and beauvericin by high-performance liquid chromatography-electrospray ionization mass spectrometry.

作者信息

Sewram V, Nieuwoudt T W, Marasas W F, Shephard G S, Ritieni A

机构信息

Programme on Mycotoxins and Experimental Carcinogenesis, Medical Research Council, Tygerberg, South Africa.

出版信息

J Chromatogr A. 1999 Oct 15;858(2):175-85. doi: 10.1016/s0021-9673(99)00814-6.

Abstract

A method is described using LC-MS for the detection of the mycotoxins fusaproliferin (FUS) and beauvericin (BEA) in cultures of Fusarium subglutinans and in naturally contaminated maize. Protonated molecular ion signals for FUS and BEA were observed at m/z 445 and m/z 784, respectively. Collision induced dissociation of the readily dehydrated protonated molecular ion of the sesterterpene FUS (m/z 427) led to the loss of another water molecule (m/z 409) and acetic acid (m/z 385), while the cyclic lactone trimer BEA fragmented to yield the protonated dimer (m/z 523) and monomer (m/z 262), respectively. Detection of FUS was best performed in the MS-MS mode while BEA displayed a stronger signal in the MS mode. The on-column instrumental detection limits for pure FUS and BEA were found to be 2 ng and 20 pg (S/N=2) while those in naturally contaminated maize were 1 microg/kg and 0.5 microg/kg, respectively. Five South African strains of F. subglutinans were analyzed following methanol extraction of which four produced FUS at levels between 330 mg/kg and 2630 mg/kg while only three produced BEA at levels between 140 mg/kg and 700 mg/kg. Application of this method to naturally contaminated maize samples from the Transkei region of South Africa showed FUS at levels of 8.8-39.6 microg/kg and BEA at 7.6-238.8 microg/kg.

摘要

本文描述了一种使用液相色谱-质谱联用(LC-MS)检测亚粘团镰刀菌培养物及天然污染玉米中霉菌毒素腐马素(FUS)和白僵菌素(BEA)的方法。分别在质荷比(m/z)445和m/z 784处观察到FUS和BEA的质子化分子离子信号。倍半萜烯FUS的易脱水质子化分子离子(m/z 427)经碰撞诱导解离,导致再失去一个水分子(m/z 409)和乙酸(m/z 385),而环状内酯三聚体BEA裂解分别产生质子化二聚体(m/z 523)和单体(m/z 262)。FUS的检测在MS-MS模式下效果最佳,而BEA在MS模式下信号更强。纯FUS和BEA的柱上仪器检测限分别为2 ng和20 pg(信噪比S/N = 2),而在天然污染玉米中的检测限分别为1 μg/kg和0.5 μg/kg。对五株南非亚粘团镰刀菌菌株进行甲醇提取后分析,其中四株产生的FUS含量在330 mg/kg至2630 mg/kg之间,只有三株产生的BEA含量在140 mg/kg至700 mg/kg之间。将该方法应用于南非特兰斯凯地区的天然污染玉米样品,结果显示FUS含量为8.8 - 39.6 μg/kg,BEA含量为7.6 - 238.8 μg/kg。

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