Ultrathin lamellar functionalized molybdenum disulfide nanocomposite material and its application in glycopeptide enrichment
A technology of molybdenum disulfide and composite materials, which is applied in the field of materials, can solve the problems of inability to analyze glycoproteins and glycopeptides, lack of versatility, difficulty in releasing sugar chain structures, etc., and achieve simple synthesis methods, increase specific surface area, Overcoming the effect of easy agglomeration
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Embodiment 1
[0068] Example 1. The enrichment and detection of glycopeptides by the functionalized molybdenum disulfide-nanogold composite material based on the principle of hydrophilic enrichment comprises the following steps:
[0069] 1. Preparation of molybdenum disulfide-nano gold:
[0070] (1) Ultrasonic dispersion of 10 mg of molybdenum disulfide powder in 1 mL of n-hexane.
[0071] (2) 3 mg of gold tetrachloride trihydrate and 100 μL of oleylamine were dissolved in 1.5 mL of n-hexane.
[0072] (3) Ultrasonic dispersion after mixing the product obtained in step (1) and the product obtained in step (2).
[0073] (4) Add 150 μL of triisopropylsilane (TIPS) to the product mixture obtained in step (3), mix well and let stand for 4 hours.
[0074] (5) Add absolute ethanol to the product obtained in step (4), mix well and centrifuge at 4,500 g for 15 minutes.
[0075] (6) Take the precipitate obtained in step (5), add n-hexane to dissolve the precipitate, then add absolute ethanol, mix ...
Embodiment 2
[0090] Example 2. Sensitivity detection of glycopeptide enrichment by functionalized molybdenum disulfide-nanogold composite material based on hydrophilic enrichment principle, including the following steps:
[0091] 1. Enrichment of glycopeptides:
[0092] (11) Weigh 1 mg of the functionalized molybdenum disulfide-nano noble metal composite material obtained in Example 1, shake and disperse it in 1 mL of enrichment buffer (acetonitrile / water / trifluoroacetic acid, 86:13.9:0.1, v / v / v) In this method, take 20 μL of the above suspension, centrifuge and remove the sediment from the lower layer, and wash 3 times with enrichment buffer.
[0093] (12) Take 100 μL enrichment buffer (acetonitrile / water / trifluoroacetic acid, 86:13.9:0.1, v / v / v), wherein the contents of IgG trypsin-digested peptides in Group 1, Group 2 and Group 3 were 6.7pmol, 20fmol and 10fmol respectively.
[0094] (13) After suspending the precipitate obtained in step (11) in the solutions of group 1, group 2 and ...
Embodiment 3
[0099]Example 3. Selective and specific detection of glycopeptide enrichment by functionalized molybdenum disulfide-nanogold composite material based on the principle of hydrophilic enrichment, including the following steps:
[0100] 1. Enrichment of glycopeptides:
[0101] (11) Weigh 1 mg of the functionalized molybdenum disulfide-nano noble metal composite material obtained in Example 1, shake and disperse it in 1 mL of enrichment buffer (acetonitrile / water / trifluoroacetic acid, 86:13.9:0.1, v / v / v) In this method, take 20 μL of the above suspension, centrifuge and remove the sediment from the lower layer, and wash 3 times with enrichment buffer.
[0102] (12) Take 100 μL enrichment buffer (acetonitrile / water / trifluoroacetic acid, 86:13.9:0.1, v / v / v), wherein the mass ratios of the mixtures each containing 2 μg of IgG and BSA digestion products in Group 1 and Group 2 were 1:200 and 1:500, respectively.
[0103] (13) After suspending the precipitate obtained in step (11) in ...
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