Methods for preparing crystalline rapamycin and for measuring crystallinity of rapamycin compounds using differential scanning calorimetry
First Claim
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1. A method for measuring particle quality of a rapamycin compound using differential scanning calorimetry, comprising:
- analyzing the heat flow signal of a sample comprising a rapamycin compound; and
comparing the heat flow signal of said sample to the heat flow signal of a predetermined standard;
wherein said particle quality is proportional to the melting temperature of said heat flow signal of said sample.
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Abstract
Methods for purifying rapamycin are described. Methods for measuring particle quality, median particle size, and crystallinity of samples containing rapamycin or a derivative thereof are also provided.
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Citations
37 Claims
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1. A method for measuring particle quality of a rapamycin compound using differential scanning calorimetry, comprising:
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analyzing the heat flow signal of a sample comprising a rapamycin compound; and
comparing the heat flow signal of said sample to the heat flow signal of a predetermined standard;
wherein said particle quality is proportional to the melting temperature of said heat flow signal of said sample. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25)
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26. A method for determining median particle size of a sample containing crystals of a rapamycin compound using differential scanning calorimetry, comprising:
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analyzing the melting temperature of a sample comprising a rapamycin compound; and
comparing the melting temperature to a predetermined standard;
wherein said median particle size is proportional to the melting temperature of said sample. - View Dependent Claims (27)
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28. A method for determining the crystallinity of a rapamycin compound, comprising:
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analyzing the heat flow signal of a test sample comprising a raparnycin compound; and
calculating the crystallinity of said test sample by comparing said heat flow signal to the heat flow signal of a predetermined standard comprising a crystalline rapamycin compound. - View Dependent Claims (29, 30, 31, 32, 33, 34, 35)
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36. A method for purifying rapamycin, comprising:
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(i) heating crude rapamycin in ethyl acetate to about 55°
C.;
(ii) filtering the product of step (i);
(iii) maintaining the temperature of step (ii) at about 54°
C. to about 57°
C.;
(iv) adding heptanes to the product of step (iii) over a period of about 60 minutes at a constant rate;
(v) maintaining the product of step (iv) at said temperature for about 30 minutes;
(vi) reducing the agitation speed of step (v);
(vii) cooling the product of step (vi) to about 40°
C. at a rate of about 5°
C./hour;
(viii) cooling the product of step (vii) to a temperature of about 25°
C. at a rate of about 7.5°
C./hour;
(ix) cooling the product of step (viii) to a temperature of about 7 to 8°
C. at a rate of at least about 9°
C./hour;
(x) maintaining the product of step (ix) at said temperature for about 2 hours; and
(xi) filtering the product of step (x) to obtain said crystalline rapamycin. - View Dependent Claims (37)
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Specification