< p > a href= "http://cailiao.sjfzxm.com/" > sensitized dye < /a > refers to certain dyes that cause skin or mucous membrane or respiratory tract allergy of human or animal, which are very harmful to human body. Many countries and world authoritative organizations have promulgated strict regulations and technical standards to restrict them.

Disperse blue 1 and disperse yellow 3 are the two representative types of sensitizing dyes. The detection methods are mainly GC-MS, liquid chromatography and liquid chromatography-mass spectrometry. Liquid chromatography tandem mass spectrometry (HPLC / MS / MS) is favored by dye analysis workers because of its high selectivity and high sensitivity.

This study provides a reliable platform for rapid detection of disperse blue 1 and disperse yellow 3 in textiles by liquid chromatography tandem mass spectrometry combined with optimized pretreatment and liquid quality conditions.

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< p > < strong > 1. the extraction conditions were optimized < /strong > < /p >.

< p > disperse blue 1 and disperse yellow 3 are easier to dissolve in organic solvents such as alcohols and ketones. The hexane, ethyl acetate, acetone and methanol are selected as the extraction reagents, and the recovery test is carried out according to the method specified in the determination of sensitized disperse dyes in GB/T 20383-2006 textiles.

The results showed that when methanol was used as the extraction reagent, the recovery rate of the two components could reach more than 85%, and the interference of impurities was less. Methanol was selected as the extraction reagent.

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< p > < strong > 2., the optimization of chromatography-mass spectrometry < /strong > < /p >

< p > < < a > href= > //m.pmae.cn/news/index_s.asp > liquid chromatography > /a > SHIMADZU LC-30 series; mass spectrometer API 4000 equipped with electrospray ion source (ESI).

The Agilent ZORBAX Extend column showed obvious advantages for the retention, sensitivity and peak type of the target, so the column was selected as the separation column.

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< p > gradient separation was carried out using acetonitrile and 5mmol/L ammonium acetate as mobile phase. The two targets were well separated and the peak type was symmetrical.

The gradient elution procedure is as follows: 0min ~ 2.5min, 15% A linear change to 95% A, 2.5min ~ 4.0min, 95%A changes linearly to 60%A, 4.0min ~ 6.0min, maintains 60%A.

Flow rate: 0.3mL/min.

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< p > 0.8 g/mL solution was used to scan the parent ions in the electrospray ionization mode under peristaltic pumping mode. The accurate molecular ions were selected as the parent ions, and the daughter ions were scanned with the molecular ions as the parent ions. The 2 sub ions with abundant abundance were selected to optimize the mass spectra parameters.

The quantitative ion was selected with large abundance and stable response.

The disperse blue 1 mother ion is 269, the quantitive ion is 107.2, the optimized taper hole voltage and the collision voltage are 115V and 50V respectively, and the taper hole voltage and the collision voltage optimized by sub ion 124.80 are 115V and 35V respectively.

The disperse yellow 3 mother ion is 270, the quantitive ion is 107.1, the optimized taper hole voltage and the collision voltage are 80V and 33V respectively, and the taper hole voltage and the collision voltage optimized by sub ion 150.2 are 80V and 25V respectively.

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< p > < strong > 3. standard curve, linear range and detection limit < /strong > < /p >

< p > according to the optimized liquid chromatography and mass spectrometry conditions, the mixed standard products with mass concentration of 0, 0.05, 0.1, 0.2, 0.4, 0.8, 1.2 g/mL were determined respectively, and the mass concentration (X, g/mL) of each component was linear regressed by the peak area (Y) of each component.

The results showed that the standard substance had a good linear relationship in the range of 0.1 g/mL to 0.8 g/mL, and the correlation coefficients were above 0.99.

SNR S/N=3 was used to calculate the detection limit of standard substance. Disperse blue 1 was 5 g/kg and disperse yellow 3 was 2.5 g/kg.

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< p > < strong > 4. recovery rate and precision analysis < /strong > < /p >

< p > 0.4 polyester g/mL mixed standard was added to polyester, cotton and chemical fiber samples. HPLC-MS/MS was determined according to the optimized extraction conditions, liquid chromatography and mass spectrometry conditions.

The results showed that the recoveries of the two certified reference materials ranged from 85.9% to 103.6%, and the relative standard deviations (RSD) ranged from 1.59% to 5.39%.

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< p > < strong > 5. conclusion < /strong > < /p >

< p > the HPLC-MS/MS method for the determination of disperse blue 1 and disperse yellow 3 in textiles was optimized by optimizing the sample pretreatment conditions and chromatography-mass spectrometry conditions.

The method has wide linear range, high sensitivity, accurate detection results, and the limit of quantification can reach 5 g/kg. It can meet the testing requirements of disperse blue 1 and disperse yellow 3 in < a href= "//m.pmae.cn/news/index_x.asp" > textiles > /a >

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