首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Simultaneous determination of multi-component mycotoxin contaminants in foods and feeds by ultra-performance liquid chromatography tandem mass spectrometry
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Simultaneous determination of multi-component mycotoxin contaminants in foods and feeds by ultra-performance liquid chromatography tandem mass spectrometry

机译:超高效液相色谱串联质谱法同时测定食品和饲料中多组分霉菌毒素污染物

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The present study developed an improved analytical method for the simultaneous quantification of 17 kinds of Aspergillus, Fusarium and Penicillium mycotoxin contaminants in foods and feeds by ultra-performance liquid chromatography combined with electrospray ionization triple quadrupole tandem mass spectrometry (UPLC-MS/MS) under the multiple reaction monitoring (MRM) mode, and especially focused on the optimization of extraction, clean-up, UPLC separation and MS/MS parameters of analytes. Homogenized samples were sequentially extracted by 84% (v/v) of acetonitrile aqueous solution with the selected internal standard (zearalanone) spiking, SPE clean-up with Mycosep 226 Aflazon+ Multifunctional cartridges, filtration, concentration and secondary filtration. Using double sample injection method, the analytes were separated by UPLC BEH C-18 column (100 mm x 2.1 mm I.D., 1.7 mu m), and eluted with ammonium acetate/methanol and aqueous ammonia/methanol for the ESI+ and ESI- analysis, respectively. The 10 positive ions and 7 negative ions of mycotoxins were separated by gradient elution with the retention time of 6.5 and 4 min, respectively. The LOQ of selected analytes ranged from 0.0 1 to 0.70 mu g kg(-1), which was lower than the criteria of EU, USA and other countries on the determination of the minimum limiting level of various mycotoxins in foods including baby foods and feed stuffs. Meanwhile, high correlation coefficients (r(2) > 0.99) of 17 mycotoxins were obtained within their respective linear ranges (0.05-20 mu g kg(-1) for 10 positive ions and 0.5-50 mu g kg(-1) for 7 negative ions) and reasonable recoveries (70.6-119.0%) of them were also demonstrated in different spiked levels. This quantitative method has many advantages including simple pretreatment, rapid determination and high sensitivity, which could be applied to the determination and quantification of multi-component mycotoxin contaminants in complex matrixes. Meanwhile, the method successfully fulfilled the minimum limiting level requests from various countries. (c) 2006 Elsevier B.V. All rights reserved.
机译:本研究开发了一种改进的分析方法,采用超高效液相色谱-电喷雾电离三重串联四极杆串联质谱(UPLC-MS / MS)同时定量分析食品和饲料中的17种曲霉,镰刀菌和青霉菌霉菌毒素污染物多反应监测(MRM)模式,尤其着重于优化分析物的提取,净化,UPLC分离和MS / MS参数。将均质化的样品依次用84%(v / v)的乙腈水溶液萃取,并带有选定的内标(玉米赤霉烯酮),用Mycosep 226 Aflazon +多功能柱纯化SPE,过滤,浓缩和二次过滤。采用双样品进样方法,通过UPLC BEH C-18色谱柱(100 mm x 2.1 mm内径,1.7μm)分离分析物,并用乙酸铵/甲醇和氨水/甲醇洗脱,进行ESI +和ESI-分析,分别。通过梯度洗脱分离真菌毒素的10个正离子和7个负离子,保留时间分别为6.5和4分钟。所选分析物的最低定量限为0.0 1至0.70μg kg(-1),低于确定包括婴儿食品和饲料在内的食品中各种霉菌毒素最低限量的欧盟,美国和其他国家/地区的标准的东西。同时,在其各自的线性范围内(10个正离子为0.05-20μg kg(-1),而对10个正离子为0.5-50μg kg(-1))获得了17种霉菌毒素的高相关系数(r(2)> 0.99)。在不同的加标水平下也显示出7个负离子)和合理的回收率(70.6-119.0%)。这种定量方法具有许多优点,包括预处理简单,快速测定和灵敏度高,可用于复杂基质中多组分霉菌毒素污染物的测定和定量。同时,该方法成功地满足了各国的最低限量要求。 (c)2006 Elsevier B.V.保留所有权利。

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