High-purity daptomycin lactone hydrolyzate and its application
A daptomycin and hydrolyzate technology, applied in the field of medical analysis, can solve the problems of large mobile phase consumption, low yield, high production cost, etc., and achieve the effects of short production cycle, high yield, and low source requirements
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Embodiment 1
[0047] 1) Alkali destruction: take 1 g of crude daptomycin, add 25ml of 0.5mol / L NaOH, wait until the sample is completely dissolved at room temperature, then add 25ml of 0.5mol / L HCl for neutralization, then add 500ml of acetonitrile-water with acetonitrile content of 50% Dilute the mixture.
[0048] 2) Refrigerate the diluted solution to 2-8°C, crystallize and precipitate overnight, and filter;
[0049] 3) Wash the filter cake with water;
[0050] 4) The filter cake was vacuum-dried at 30°C to obtain 530 mg of pure daptomycin lactone hydrolyzate, with a normalized content of 97.16%, see figure 1 .
[0051] The full amino acid sequence of the hydrolyzate of daptomycin lactone was tested by positive ion mode mass spectrometry, and the full amino acid sequence of the hydrolyzate was as follows:
[0052] Dec-Trp(1)-Asn(2)-Asp(3)-Thr(4)-Gly(5)-Orn(6)-Asp(7)-Ala(8)-Asp(9)-Gly(10 )-Ser(11)-3mGlu(12)-Kyn(13).
[0053] The proton nuclear magnetic resonance spectrum of the daptom...
Embodiment 2
[0055] 1) Alkali destruction: Take 10g of daptomycin finished product, add 150ml 1mol / L NaOH, wait until the sample is completely dissolved at room temperature, then add 150ml 1mol / L HCl for neutralization, then add 3800ml of acetonitrile-water mixture with 70% acetonitrile content dilution.
[0056] 2) Refrigerate the diluted solution to 2-8°C, crystallize and precipitate overnight, and filter.
[0057] 3) Wash the filter cake with water.
[0058] 4) The filter cake was vacuum-dried at 30° C. to obtain 5.02 g of pure daptomycin lactone hydrolyzate, with a normalized content of 96.15%.
[0059] The complete amino acid sequence and H NMR spectrum of the daptomycin lactone hydrolyzate prepared in this example are the same as those in Example 1.
Embodiment 3
[0061] 1) Alkali destruction: take 1g of daptomycin powder for injection, add 50ml of 0.01mol / L KOH, wait until the sample is completely dissolved at room temperature, then add 50ml of 0.01mol / L HCl for neutralization, and then add 500ml of acetonitrile- Dilute with water mixture.
[0062] 2) Refrigerate the diluted solution to 2-8°C, crystallize and precipitate overnight, and filter.
[0063] 3) Wash the filter cake with water.
[0064] 4) The filter cake was vacuum-dried at 30° C. to obtain 503 mg of pure daptomycin lactone hydrolyzate, with a normalized content of 96.65%.
[0065] The complete amino acid sequence and H NMR spectrum of the daptomycin lactone hydrolyzate prepared in this example are the same as those in Example 1.
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