首页>
外国专利>
PROCEDURE FOR THE IDENTIFICATION AND QUANTIFICATION OF THE GLYPHOSATE PRODUCT AND THE METABOLITE OF THE AMINO-METHYL PHOSPHONIC ACID DIRECTLY FROM HONEY, USING AN ANALYTIC EXTRACTION FOLLOWED BY A LIQUID CHROMATOGRAPHY COUPLED TO MASS SPECTROMETRY.
PROCEDURE FOR THE IDENTIFICATION AND QUANTIFICATION OF THE GLYPHOSATE PRODUCT AND THE METABOLITE OF THE AMINO-METHYL PHOSPHONIC ACID DIRECTLY FROM HONEY, USING AN ANALYTIC EXTRACTION FOLLOWED BY A LIQUID CHROMATOGRAPHY COUPLED TO MASS SPECTROMETRY.
The present disclosure is related to a new procedure for the identification and quantification of glyphosate found in honey using a liquid chromatography technique coupled to mass spectrometry. The aim of the present invention is to obtain the necessary information to approve the purity of honey within the maximum limits of foreign matter and chemical contaminants, and reduce the risk for consumers. The proposed procedure is based on the determination of glyphosate along with its metabolite, whose residues appear due to the enormous proliferation of the same in agriculture and which were previously poorly evaluated. Comprises a sequence of five stages: A first stage, consisting of a dilution in all samples including fortified samples for the honey curve, then the samples are taken to an incubation process. A second stage that consists in adjusting the pH to a value of between 2.5-3.5, by means of an organic acid. A third step, centrifuging the samples prior to loading the samples to an OASIS PRIME HLB column, followed by elution, the sample is subjected to total dryness in the presence of nitrogen in a bain-marie. A fourth step, consisting of the addition of an ammonium acetate solution, in order to reconstitute with 300 ml, filter through a 0.45 µm acrodisk and transfer to a vial with insert. Finally, the samples are injected into a liquid chromatography device coupled to mass spectrometry, whose parameters are set according to the established tables. Therefore, the scope of the invention is determined within the universe of glyphosate determination and amino methyl phosphonic acid obtaining certainty by analyzing liquid chromatography coupled to mass spectrometry and thereby determining the residues contained in honey.
展开▼
机译：本公开涉及使用与质谱联用的液相色谱技术鉴定和定量蜂蜜中发现的草甘膦的新方法。本发明的目的是获得必要的信息，以在最大的异物和化学污染物极限内批准蜂蜜的纯度，并降低消费者的风险。拟议的程序基于草甘膦及其代谢物的测定，其残留物是由于其在农业中的大量繁殖而出现的，并且以前没有得到很好的评估。包括五个阶段的序列：第一阶段，包括对所有样品进行稀释（包括用于蜂蜜曲线的强化样品），然后将样品送入培养过程。第二阶段包括通过有机酸将pH调节至2.5-3.5之间的值。第三步，在将样品上样至OASIS PRIME HLB色谱柱之前先对样品进行离心，然后进行洗脱，然后在贝恩-玛丽实验室中在氮气存在下对样品进行完全干燥。第四步，包括添加乙酸铵溶液，以便用300 ml复溶，通过0.45 µm杂花盘过滤，然后转移到带有插入物的小瓶中。最后，将样品注入与质谱联用的液相色谱仪中，其参数根据已建立的表格进行设置。因此，本发明的范围是在草甘膦测定和氨基甲基膦酸通过分析与质谱联用的液相色谱法并由此确定蜂蜜中所含残留物而确定的范围内确定的。
展开▼
