Method for simultaneously screening and analyzing forbidden and restricted dye in textiles

Abstract

The invention discloses a method for simultaneously screening and analyzing forbidden and restricted dye in textiles. The method includes steps of (1), stripping colors of samples and extracting the samples to obtain extract liquid; (2), separating the samples by the aid of reversed phase liquid chromatograms, measuring the samples by the aid of high-resolution mass spectra and acquiring data of chromatogram peak retention time, accurate mass numbers of parent ions, isotope distribution of the parent ions and the like; (3), screening and analyzing the samples, to be more specific, determining that the samples are positive samples if high-resolution mass spectrum data of the samples simultaneously meet conditions, or determining that the samples are negative samples if the high-resolution mass spectrum data of the samples do not simultaneously meet the conditions, quantitatively analyzing the samples, to be more specific, extracting the accurate mass numbers of the parent ions of the samples, computing chromatogram peak areas, comparing the chromatogram peak areas to chromatogram peak areas of standard solution and quantitatively analyzing the samples. The conditions include that the allowable deviation of the retention time is + / -0.2 min, the allowable deviation of the accurate mass numbers of the parent ions is + / -5 ppm, and matching threshold values of the isotope distribution of the parent ions are larger than 70%. The method has the advantages that the samples are treated in such detection modes that the samples are treated at one step and are injected at one step and multiple compound analysis results are obtained at one step, accordingly, the detection efficiency can be greatly improved, and the detection cost can be reduced; the method is simple, convenient and speedy and is high in recycling rate and operability.

Description

technical field [0001] The invention relates to a screening method for prohibited and restricted dyes in textiles, in particular to a detection method for simultaneously screening and analyzing 42 prohibited and restricted dyes in textiles by high-resolution mass spectrometry, and belongs to the technical field of analytical chemistry. Background technique [0002] Since July 15, 1994, when the German government promulgated the ban on certain dyes, with the continuous improvement of health and ecological protection requirements in various countries, the scope of banned and restricted dyes in textiles has continued to expand. Many countries and regions, including my country, have The laws and regulations on the prohibition and restriction of relevant dyes have been issued successively, mainly including "GB / T 18885-2009 Technical Requirements for Ecological Textiles", "Oeko-Tex Standard 100 International Ecological Textile Standard", "RSL (Restricted Substances List) Restricted ...

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Problems solved by technology

[0003] At present, there are three main problems in the detection of prohibited and restricted dyes in textiles: First, the existing literature and detection standards mostly use high-performance liquid chromatography (HPLC-DAD), liquid chromatography-mass spectrometry (LC-MS), liquid chromatography Chromatography-tandem mass spectrometry (LC-MS / MS) and other methods, in which chromatographic analysis, for substances with complex compositions and large quantities such as chemical dyes, cannot be simultaneously analyzed and determined by multiple components due to separation difficulties, but based on low-resolution mass spectrometry Both LC-MS and LC-MS / MS mass spectrometry are used to classify and group dyes. Multiple tests on the same sample are required to cover the range of dye substances involved in regulations. The detection process is cumbersome, long-term, and high-cost; 2. Dye-related regulations, such as Oeko, RSL, SVHC, etc. have been updated frequently in recent years, and the number of prohibited and restricted dye compounds has been increasing. Traditional technology can only passively develop methods for specific targets, and cannot carry out dyes without standard products in textiles. Qualitative and fast screening of substances, it is impossible to backtrack the results of the expansion of the range of compounds on the measured samples, resulting in detection technology that lags behind the restrictive regulations; third, some banned and restricted chemical dyes have no specific compound information in the regulations, and due to synthetic process problems, Dyes and even dye standard substances usually contain quite a lot of impurities, which leads to unknown or even wrong analysis targets during the detection process. There are difficulties in the qualitative aspects of compounds, and false positives and false negatives are easy to appear in the test results.

In recent years, high-resolution mass spectrometry has been gradually applied in food testing, proteomics, etc., but the detection of banned and restricted dyes in textiles is still blank, and there is no simultaneous screening analysis covering more than 40 kinds of banned and restricted dyes in major regulations. Dye reports

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