高效液相色谱-三重四级杆质谱法同时测定大米中的伏马毒素B1、B2、B3

doi:10.3969/j.issn.1006-3110.2017.03.035

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摘要目的建立高效液相色谱-三重四级杆质谱法同时测定大米中的伏马毒素B₁、B₂、B₃。方法大米样品经乙腈:水=50:50提取,以Multistep@211 Fum柱进行净化,将洗脱液氮吹至干,加1.0 ml 0.2%甲酸/乙腈=65:35溶解并定容, 用LC-MS/MS检测。结果待测组分在5~800 ng/ml范围内呈现良好的线性关系,相关系数均大于0.9996,检测限介于0.045~0.10 ng/ml。以空白大米粉样品进行加标水平分别为20、100、400 ng/g的回收率实验,回收率在 94.5%~110.5%之间。结论该方法快速、准确,适用于大米中伏马毒素的测定。

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	陈丽惠
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关键词 ：伏马毒素, 高效液相色谱, 三重四级杆质谱, 大米

Abstract：Objective To establish a method for simultaneous determination of fumonisins B₁, B₂ and B₃ in rice by high-performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC-TQMS). Methods The fumonisins were extracted with 50% acetonitrile in a water bath, and purified by Multistep@211 Fum extraction cartridge. The eluate was concentrated to dryness, and dissolved with 1.0 ml 0.2% formic acid /acetonitrile=65:35, and then detected by HPLC-TQMS. Results Target compounds presented a good linear relationship in the range of 5-800 ng/ml. The correlation coefficients were larger than 0.9996 and the limits of detection were in the range of 0.045-0.10 ng/ml. The recoveries of standard addition for spiked samples in 20 ng/g,100 ng/g, and 400 ng/g were between 94.5%-110.5%. Conclusions The proposed method is rapid, accurate and suitable for determining fumonisins in rice.

Key words： fumonisin high performance liquid chromatography triple quadrupole mass spectrometry rice

收稿日期: 2016-10-09

R155.5

基金资助:2016 年福建省科技项目(NO.2016D022)

通讯作者: 贾玉珠, E-mail:jiayuzhu64@163.com。

作者简介: 陈丽惠(1985-),女,福建厦门人,硕士,研究方向:食品理化检测。

引用本文:

陈丽惠, 蔡伟鹏, 白艳艳, 朱宝平, 贾玉珠. 高效液相色谱-三重四级杆质谱法同时测定大米中的伏马毒素B₁、B₂、B₃[J]. 实用预防医学, 2017, 24(3): 375-377. CHEN Li-hui, CAI Wei-peng, BAI Yan-yan, ZHU Bao-ping, JIA Yu-zhu. Simultaneous determination of fumonisins B₁, B₂ and B₃ in rice y high-performance liquid chromatography-triple quadrupole mass spectrometry. , 2017, 24(3): 375-377.

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