Crystal Forms of Demethyleneberberine Hydrochloride and Preparation Method Therefor

A crystal form of demethyleneberberine hydrochloride selected from:

• A) a crystal form designated as crystal form A, characterized in that, it has characteristic diffraction peaks at 6.838, 8.300, 12.477, 13.667, 16.269, 16.642, 17.761, 18.247, 18.749, 20.389, 20.739, 21.926, 22.530, 23.983, 24.819, 25.774, 26.413, 26.592, 28.552, 30.333, and 38.312° in an X-ray powder diffraction spectrum represented by Cu-Kα radiation and 20±0.2° diffraction angle;
• one thermal absorption peak at 240±3° C. in a DSC thermogram;
• and characteristic infrared absorption peaks at 422.8 cm−1, 454.3 cm−1′, 466.6 cm−1, 505.6 cm−1, 581.8 cm−1, 617.7 cm−1, 658.5 cm−1, 739.3 cm−1, 774.6 cm−1, 820.3 cm−1, 871.8 cm−1, 892.6 cm−1, 917.5 cm−1, 962.6 cm−1, 983.2 cm−1, 999.7 cm−1, 1,050.0 cm−1, 1,067.8 cm−1, 1,110.5 cm−1, 1,140.5 cm−1, 1,203.4 cm−1, 1,244.5 cm−1, 1,268.1 cm−1, 1,293.8 cm−1, 1,337.1 cm−1, 1,363.8 cm−1, 1,390.5 cm−1, 1,455.5 cm−1, 1,493.9 cm−1, 1,515.6 cm−1, 1,530.5 cm−1, 1,567.1 cm−1, 1,605.6 cm−1, 1,638.0 cm−1, 1,769.6 cm−1, 2,726.3 cm−1, 2,847.6 cm−1, 2,945.2 cm−1, 3,024.2 cm−1, 3,065.1 cm−1, 3,086.0 cm−1, and 3,150.6 cm−1;
• B) a crystal form designated as crystal form B, characterized in that, it has characteristic diffraction peaks at 6.838, 8.300, 12.477, 13.667, 16.269, 16.642, 17.761, 18.247, 18.749, 20.389, 20.739, 21.926, 22.530, 23.983, 24.819, 25.774, 26.413, 26.592, 28.552, 30.333, and 38.312° in an X-ray powder diffraction spectrum represented by Cu-Kα radiation and 2θ±0.2° diffraction angle:
• two thermal absorption peaks at 147±3° C. and 220±3° C. respectively in a DSC thermogram;
• and characteristic infrared absorption peaks at 421.5 cm−1, 448.0 cm−1, 464.4 cm−1, 506.1 cm−1, 523.9 cm−1, 543.5 cm−1, 568.8 cm−1, 583.9 cm−1, 618.9 cm−1, 649.1 cm−1, 676.8 cm−1, 718.3 cm−1, 742.1 cm−1, 777.5 cm−1, 833.0 cm−1, 859.8 cm−1, 878.7 cm−1, 924.5 cm−1, 960.4 cm−1, 977.7 cm−1, 1,018.9 cm−1, 1,060.0 cm−1, 1,107.7 cm 1,138.4 cm−1, 1,170.1 cm−1, 1,207.4 cm−1 1,243.9 cm−1, 1,268.6 cm−1, 1.366.8 cm−1, 1,388.7 cm−1 1,422.7 cm−1, 1,445.5 cm−1, 1,457.3 cm−1, 1,492.8 cm−1, 517.8 cm−1, 1,533.9 cm−1, 1,568.8 cm−1, 1,610.9 cm−1, 1,636.9 cm−1, 1,735.5 cm−1, 2,646.6 cm−1, 2,849.8 cm−1, 2,952.5 cm−1, 2,993.5 cm−1, 3,089.6 cm−1, and 3,364.3 cm−1;
• C) a crystal form designated as crystal form C, characterized in that, it has characteristic diffraction peaks at 3.260, 8.515, 9.715, 12.147, 13.219, 14.789, 17.607, 18.306, 20.728, 21.261, 24.633, 25.430, 25.837, 26.416, 27.606, 28.147, and 37.695° in an X-ray powder diffraction spectrum represented by Cu-Kα radiation and 2θ±0.2° diffraction angle:
• one thermal absorption peak at 253±3° C. in a DSC thermogram;
• and characteristic infrared absorption peaks at 422.8 cm−1, 441.6 cm−1, 452.2 cm−1, 505.0 cm−1, 526.2 cm−1, 584.6 cm−1, 637.3 cm−1, 652.0 cm−1, 665.7 cm−1, 699.9 cm−1, 723.4 cm−1, 742.0 cm−1, 774.1 cm−1, 814.2 cm−1, 828.2 cm−1, 869.6 cm−1, 891.7 cm−1, 915.6 cm−1, 964.5 cm−1, 980.6 cm−1, 998.8 cm−1, 1,065.8 cm−1, 1,108.5 cm−1, 1,139.7 cm−1, 1,192.2 cm−1, 1,216.5 cm−1, 1,241.0 cm−1, 1.273.9 cm−1, 1,287.4 cm−1, 1,308.2 cm−1, 1,343.5 cm−1, 1,356.5 cm−1, 1,389.3 cm−1, 1,420.2 cm−1, 1,437.9 cm−1, 1,456.1 cm−1, 1,510.2 cm−1, 1,565.5 cm−1, 1,580.9 cm−1, 1,604.3 cm−1, 1.618.6 cm−1, 1.633.2 cm−1, 2,697.9 cm−1, 2,842.7 cm−1, 2,946.1 cm−1, 3,005.3 cm−1, and 3,066.4 cm−1;
• and
• D) a crystal form designated as crystal form D, characterized in that, it has characteristic diffraction peaks at about 6.034, 8.699, 12.589, 18.108, 21.854, 24.224, 25.146 and 26.172° in an X-ray powder diffraction spectrum represented by Cu-Kα radiation and 2 diffraction angle:
• two thermal absorption peaks at 131±3° C. and 190±3° C. respectively in a DSC thermogram;
• and characteristic infrared absorption peaks at 422.8 cm−1, 454.3 cm−1, 466.6 cm−1, 505.6 cm−1, 581.8 cm−1, 617.7 cm−1, 658.5 cm−1, 739.3 cm−1, 774.6 cm−1, 820.3 cm−1, 871.8 cm−1, 892.6 cm−1, 917.5 cm−1, 962.6 cm−1, 983.2 cm−1, 999.7 cm−1, 1,050.0 cm−1, 1,067.8 cm−1, 1,110.5 cm−1, 1,140.5 cm−1, 1,203.4 cm−1, 1,244.5 cm−1, 1,268.1 cm−1, 1,293.8 cm−1, 1,337.1 cm−1, 1,363.8 cm−1, 1,390.5 cm−1, 1,455.5 cm−1, 1,493.9 cm−1, 1,515.6 cm−1, 1,530.5 cm−1, 1.567.2 cm−1, 1,605.6 cm−1, 1,638.0 cm−1, 1,769.6 cm−1, 2,726.3 cm−1, 2,847.6 cm−1, 2,945.2 cm−1, 3,024.2 cm−1, 3,065.1 cm−1, 3,086.0 cm−1, and 3,150.6 cm−1.