Preparation method and application of a high-selectivity solid-phase microextraction probe for triphenylmethane dye and its metabolites
A metabolite, triphenylmethane technology, applied in the field of micro-extraction electrospray probe, achieves the effect of mild preparation conditions, good reproducibility and stability, and suppression of matrix interference
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Embodiment 1
[0028] A novel SPME probe is prepared by the following steps:
[0029] (1) First use 30% (wt / wt) sulfuric acid solution containing 30mg mL-1 potassium permanganate and 15mg mL-1 potassium dichromate and tungsten needle to reflux at 90°C for 5 days, then oxidize with hydrogen The sodium solution and the tungsten needle were refluxed at 90°C for 5 days, then washed with methanol, and dried with nitrogen at room temperature;
[0030] (2) Put the tungsten needle treated in (1) into a double-necked flask, add 50mL of anhydrous N,N-dimethylformamide and 2.5mL of trimethoxy(4-vinylphenyl)silane, and Into nitrogen, heated to 120 ° C reflux reaction for 12h. After the reaction is completed, the tungsten needle with the silylating agent bonded on the surface is washed three times with methanol, and dried with nitrogen at room temperature;
[0031] (3) Put the dried tungsten needle in (2) in 3M sodium metabisulfite solution (sodium hydroxide adjusts the pH to 6.5), and react under nitr...
Embodiment 2
[0033] Research on the experimental conditions of the SPME probe prepared in Example 1.
[0034] Firstly, a series of extraction times such as 10, 20, 40, 60, 120, 180, 300s were investigated. from image 3 In middle a), it can be seen that as the extraction time increases, the signal strength gradually increases until it reaches a plateau over 60s, and the longer extraction time does not significantly increase the signal strength. On the other hand, since in vivo analysis will be carried out later, the extraction time should not be too long, so 60s is taken as the optimal extraction time.
[0035] The present invention has studied the extraction result of multiple desorption solvents simultaneously ( image 3 In b)), including methanol, acetonitrile, methanol / water (v / v=1:1) and acetonitrile / water (v / v=1:1), as can be seen from the figure, when the desorption solvent is methanol When the signal intensity was the best, methanol was finally selected as the desorption solvent...
Embodiment 3
[0037] Under the optimum experimental condition determined in embodiment 2, explored the extraction performance and the quantitative ability of the SPME probe prepared in embodiment 1, specifically comprise the following steps:
[0038]Transfer two grams of homogenized fish flesh to a clean 10-ml glass tube, then add 2 ml of deionized water and mix for 10 minutes. Add 99 μL of fish meat to 1 μL of MG, CV, LMG and LCV standard solutions (methanol / water less than 1:9, v / v) to form a series of concentrations at 0.1, 0.5, 1, 5 and 10 ng mL -1 standard sample.
[0039] Deuterated malachite green (abbreviated as d 5 -MG), deuterated crystal violet (abbreviated as d 6 -CV), deuterated leuco malachite green is abbreviated as (d 6 -LMG) and deuterated leuco malachite green (abbreviated as d 6 -LCV) was added to the spray solvent as 1 ng mL -1 Isotopic internal standard compounds at concentration levels. The internal standard compound is used for error calibration in the analysis ...
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