Glycometabolism labeling probe, kit containing same and application thereof
A technology for labeling probes and sugar metabolism, applied in biological testing, microbial determination/inspection, instruments, etc. effect of reaction
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Embodiment 1
[0068] Example 1: 1,3-Ac 2 GalNAz and 1,3-Pr 2 Synthesis of GalNAz
[0069] (A)1,3-Ac 2 The synthesis of GalNAz sees following route (I):
[0070]
[0071] Among them, the conditions of steps a, b and c are respectively:
[0072] Under ice bath, GalNAz (Compound 1, 200 mg, 0.76 mmol) was suspended in 5 mL of acetone, 2,2-dimethoxypropane (0.94 mL, 763 mmol) was added dropwise, and finally camphorsulfonic acid (17.7 mg , 7.63 mmol). The system was slowly raised to 4°C, and stirring was continued for 1h. The reaction was quenched with triethylamine, the solvent was spin-dried, and purified with a silica gel column (ethyl acetate:petroleum ether rose from 1:1 to 4:1) to obtain a white crude product (R f =0.2, ethyl acetate). The product was further purified by HPLC to give a white product (110 mg, 48%, α / β=3:1).
[0073] Its NMR test data are: 1 H NMR (500MHz, CD 3 OD)δ5.23(d,J=3.5Hz,1H),4.67(d,J=8.5Hz,1H),4.33(dd,J=11.0,3.5Hz,1H),4.28(d,J=4.0, 1H),4.24-4.16(m,3H),4...
Embodiment 2
[0088] Example 2 1,3-Ac 2 GalNAz and 1,3-Pr 2 In vitro reaction of GalNAz with protein
[0089] In order to verify 1,3-Ac 2 GalNAz and 1,3-Pr 2 GalNAz cannot spontaneously react with protein cysteine. With unprotected GalNAz as a positive control and fully protected Ac4GalNAz as a negative control, the above two probes were mixed with different cell protein lysates (cell lysates) or single protein After incubation at 37° C. for 2 h, the azide signal on the protein was detected by electrophoresis gel.
[0090] The result is as follows Figure 2a to Figure 2e As shown, among them, Figure 2a Shown is 1,3-Ac 2 GalNAz and 1,3-Pr 2 The detection results of the reaction of two GalNAz probes with the protein lysate of Hela cells; Figure 2b Shown is 1,3-Ac 2 GalNAz and 1,3-Pr 2 The detection results of the reaction of two GalNAz probes to the protein lysate of 293T cells; Figure 2c Shown is 1,3-Ac 2 GalNAz and 1,3-Pr 2 The detection results of GalNAz two probes reacting t...
Embodiment 3
[0092] Example 3 In vivo metabolic labeling effect
[0093] In order to verify its metabolic labeling effect in vivo, the above-mentioned 1,3-Ac 2 GalNAz and 1,3-Pr 2 GalNAz probes for metabolic labeling of HeLa cells. The specific operation steps are:
[0094] 100μM, 200μM, 1mM 1,3-Ac 2 GalNAz, 100 μM, 200 μM 1,3-Ac 2 GalNAz1,3-Pr 2 GalNAz and 200μM and 1mM GalNAz probes were added to the culture medium of Hela cells for culture, and then through bio-orthogonal reaction with Cy5 fluorescently labeled substances, the in-gel fluorescence detection was performed on HeLa cells after different treatments, and the detection results See image 3 ( image 3 CBB in indicates Coomassie Brilliant Blue staining to show loading control).
[0095] From image 3 It can be seen that 100 μM 1,3-Pr 2 The metabolic labeling efficiency of GalNAz is equivalent to or even exceeds the labeling effect of 1mM GalNAz (while Ac 4 GalNAz labeling has side effects, due to false positive labeli...
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