Method for analyzing sulfonamide substances by magnetic solid-phase extraction and isotope dimethyl mark
A dimethylation and isotope technology, which is applied in the field of magnetic solid-phase extraction combined with isotope dimethylation labeling to analyze sulfonamide substances, can solve the problems of difficult to obtain the price of isotope internal standard, difficult to realize quantitative analysis, etc., and achieve high efficiency and selectivity. The effect of enrichment, improving labeling efficiency and saving dosage
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Embodiment 1
[0030] Embodiment 1: the analysis of sulfa compound in tap water
[0031] 1) Take 1mL of the water sample to be tested, directly measure the total nitrogen without filtering, and calculate the required labeling reagent CD according to the total nitrogen of the sample 2 The consumption of O, its consumption is 50 times (mol ratio) of total nitrogen;
[0032] 2) Take 200mL of the water sample to be tested and add 20mg of the same amount of magnetic carbon nanomaterials (washed three times with acetonitrile and balanced once with ultrapure water) to the water sample A to be tested and the equal volume (0.1μg / L) of sulfonamide mixed standard solution B In, shaking to complete the adsorption and enrichment of sulfa substances;
[0033] 3) Magnetic separation under an external magnetic field, pour off the residual liquid after adsorption, transfer the magnetic carbon nanomaterials that have been adsorbed to 1.5mL centrifuge tubes, add 0.5mL of 50mM sodium phosphate buffer solution (p...
Embodiment 2
[0037] Embodiment 2: the analysis of sulfa compound in river water
[0038] 1) Take river water with different sections and depths, mix and let stand for 1 hour to make the sediment and water preliminarily separate under the action of gravity, take the supernatant (volume greater than 150mL) and filter it as the water sample to be tested;
[0039] 2) Take 1mL of the filtered water sample to be tested, measure its total nitrogen, and calculate the required labeling reagent CH according to the total nitrogen of the sample. 2 The consumption of O, its consumption is 50 times (mol ratio) of total nitrogen;
[0040] 3) Take 100mL of the filtered water sample to be tested, add the same amount of magnetic carbon nanomaterials 50mg (washed three times with acetonitrile, and balance once with ultrapure water) to the water sample A to be tested and an equal volume (1μg / L) of sulfonamide In the mixed standard solution B, shake to complete the adsorption of sulfa substances;
[0041] 4)...
Embodiment 3
[0045] Example 3: Analysis of sulfa compounds in milk
[0046] 1) Take 10 mL of milk sample into a 50 mL centrifuge tube, add 0.5 g of hydroxylamine hydrochloride, vortex and mix well, add 25 mL of ethyl acetate, cover tightly and shake on a shaker (100 r / min) for 20 min;
[0047] 2) Centrifuge (4000r / min), transfer the supernatant to a rotary evaporator and evaporate to dryness (33°C±2°C);
[0048] 3) Dissolve the residue with 10mL of 1% phosphoric acid solution, add 5mL of n-hexane, vortex mix for 2min, let it stand for 10min, remove the n-hexane layer and transfer to a rotary evaporator to evaporate to dryness;
[0049] 4) Redissolve the residue after evaporation to dryness with 10mL 20% methanol solution, as sample A to be tested;
[0050] 5) Take 0.1 mL of sample A, dilute it to 1 mL with water, measure its total nitrogen, and then convert it to obtain the total nitrogen in sample A. According to the total nitrogen in sample A, calculate the required labeling reagent CH...
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