CN101033211A - 5-氯-4-羟基-2(1h)-吡啶酮晶型及其制备方法和应用 - Google Patents
5-氯-4-羟基-2(1h)-吡啶酮晶型及其制备方法和应用 Download PDFInfo
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- CN101033211A CN101033211A CN 200710020907 CN200710020907A CN101033211A CN 101033211 A CN101033211 A CN 101033211A CN 200710020907 CN200710020907 CN 200710020907 CN 200710020907 A CN200710020907 A CN 200710020907A CN 101033211 A CN101033211 A CN 101033211A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
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- 239000013078 crystal Substances 0.000 claims abstract description 144
- 206010028980 Neoplasm Diseases 0.000 claims abstract description 17
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- UBQKCCHYAOITMY-UHFFFAOYSA-N pyridin-2-ol Chemical compound OC1=CC=CC=N1 UBQKCCHYAOITMY-UHFFFAOYSA-N 0.000 claims description 17
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Images
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Abstract
Description
晶面d-间距(_) | 相对强度(I/I0) |
5.93 | 59 |
4.79 | 27 |
3.46 | 100 |
3.42 | 35 |
3.24 | 61 |
2.97 | 16 |
2.77 | 22 |
晶面间距d值(_) | 相对强度(I/I0) |
6.25 | 5 |
5.93 | 59 |
4.79 | 27 |
4.57 | 9 |
4.29 | 9 |
3.63 | 9 |
3.46 | 100 |
3.42 | 35 |
3.24 | 61 |
3.16 | 8 |
3.13 | 12 |
2.97 | 16 |
2.88 | 10 |
2.77 | 22 |
2.60 | 6 |
2.43 | 8 |
2.37 | 13 |
2.21 | 7 |
2.08 | 9 |
2.00 | 5 |
1.87 | 7 |
晶面间距d值(_) | 相对强度(I/I0) |
8.62 | 59 |
8.26 | 100 |
4.90 | 69 |
4.70 | 35 |
2.88 | 24 |
2.75 | 43 |
晶面间距d值(_) | 相对强度(I/I0) |
14.6 | 11 |
8.62 | 59 |
8.26 | 100 |
7.34 | 13 |
7.03 | 6 |
5.63 | 21 |
5.45 | 19 |
5.38 | 20 |
4.90 | 69 |
4.70 | 35 |
3.68 | 18 |
3.59 | 5 |
3.53 | 9 |
3.42 | 19 |
3.26 | 15 |
2.95 | 7 |
2.88 | 24 |
2.82 | 9 |
2.75 | 43 |
2.67 | 8 |
2.45 | 9 |
2.13 | 9 |
2.06 | 11 |
保留时间 | 峰面积% | 峰面积 | 峰分离度 |
3.4844.2915.4539.66811.886 | 0.058850.17850.0344899.690.0433 | 9311282385456157722776851 | 2.583.917.195.260.00 |
100 | 15822132 |
保留时间 | 峰面积% | 峰面积 | 峰分离度 |
3.5674.3435.5089.83812.127 | 0.038230.29120.131899.50.03955 | 60094577220720156414116217 | 2.364.157.555.460.18 |
100 | 15720129 |
保留时间 | 峰面积% | 峰面积 | 峰分离度 |
3.6594.3115.4409.65312.003 | 0.052630.16130.0232199.730.03902 | 8275253543650156805656136 | 2.209.707.485.600.00 |
100 | 15723980 |
保留时间 | 峰面积% | 峰面积 | 峰分离度 |
4.3405.4769.78312.203 | 0.24360.113299.620.01818 | 3642816920148952802718 | 3.777.560.000.00 |
100 | 14951347 |
胶囊批号 | 溶出量(%) | |||||
5min | 10min | 20min | 30min | 45min | 60min | |
040706-1(含P晶型) | 52.6 | 70.7 | 97.5 | 98.4 | 98.1 | 97.4 |
040706-2(含L晶型) | 50.3 | 68.8 | 97.7 | 98.0 | 99.3 | 98.2 |
时间(h) | 8 | 9 | 10 | 11 | 12 | 13 | 14 | mean | s |
0.0830.250.500.751234 | 0.3150.9901.3051.3531.2250.6540.4860.188 | 0.3161.0491.5731.8911.9580.7370.3500.137 | 0.5491.2661.6741.7211.6170.9050.3920.183 | 0.5070.9751.2201.5181.9751.0590.5070.349 | 0.3531.4971.7391.7711.9091.0740.5720.402 | 0.4011.2081.5041.6011.1620.8250.4720.254 | 0.3901.2501.7101.8521.7031.0180.5310.247 | 0.4051.1771.5321.6721.6500.8960.4730.251 | 0.0910.1870.2030.1930.3390.1640.0780.095 |
68 | 0.1470.124 | 0.1170.082 | 0.1830.152 | 0.1440.101 | 0.1470.095 | 0.2100.139 | 0.1400.101 | 0.1560.113 | 0.0310.026 |
时间(h) | 1 | 2 | 3 | 4 | 6 | 7 | mean | s |
0.0830.250.500.75123468 | 0.2380.8501.3721.5971.8461.2300.5150.3200.1580.137 | 0.3770.9031.4591.7791.9491.2670.4720.2520.1410.110 | 0.1820.9611.2781.4001.2030.7180.4090.2170.1640.054 | 0.2210.8471.0641.4311.1780.8860.3720.1900.1090.081 | 0.2091.0781.4551.5671.4340.7840.5260.2380.1900.068 | 0.4281.0141.3071.4631.5740.7210.5220.3750.1870.099 | 0.2760.9421.3221.5391.5310.9340.4700.2650.1580.092 | 0.1010.0930.1470.1400.3220.2510.0650.0690.0300.030 |
参数 | 单位 | 8 | 9 | 10 | 11 | 12 | 13 | 14 | Mean | SD |
AUC0→8AUC0→∞CmaxTmaxMRTT1/2CL | μg.h/mlμg.h/mlμg/mlhhhL/h/kg | 3.523.961.350.754.772.472.53 | 3.964.201.961.003.962.052.38 | 4.284.871.720.754.912.682.05 | 4.674.931.971.003.701.802.03 | 5.065.301.911.003.611.701.89 | 4.044.551.600.754.742.532.20 | 4.574.831.850.753.731.842.07 | 4.304.661.770.864.202.152.16 | 0.510.460.230.130.580.400.22 |
参数 | 单位 | 1 | 2 | 3 | 4 | 6 | 7 | Mean | SD |
AUC0→8AUC0→∞CmaxTmaxMRTT1/2CL | μg.h/mlμg.h/mlμg/mlhhhL/h/kg | 4.785.171.851.003.911.981.93 | 4.775.061.951.003.601.821.98 | 3.483.611.400.753.651.742.77 | 3.413.621.430.753.671.842.76 | 4.024.191.570.753.751.802.38 | 4.224.521.571.004.182.082.21 | 4.114.361.630.883.791.882.34 | 0.600.680.220.140.220.130.37 |
CD040608P | CD040608L | ||||
参数 | 单位 | Mean | SD | Mean | SD |
AUC0→8AUC0→∞CmaxTmaxMRTT1/2CL | μg.h/mlμg.h/mlμg/mlhhhL/h/kg | 4.304.661.770.864.202.152.16 | 0.510.460.230.130.580.400.22 | 4.114.361.630.883.791.882.34 | 0.600.680.220.140.220.130.37 |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103159673A (zh) * | 2011-12-12 | 2013-06-19 | 山东新时代药业有限公司 | 一种制备吉美嘧啶的精制方法 |
CN103694165A (zh) * | 2013-11-12 | 2014-04-02 | 江苏正大清江制药有限公司 | 吉美嘧啶无定形固化物及制备方法 |
CN104496972A (zh) * | 2014-12-04 | 2015-04-08 | 浙江大学 | 一种新型替加氟药物共晶及其制备方法 |
-
2007
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103159673A (zh) * | 2011-12-12 | 2013-06-19 | 山东新时代药业有限公司 | 一种制备吉美嘧啶的精制方法 |
CN103159673B (zh) * | 2011-12-12 | 2015-02-04 | 山东新时代药业有限公司 | 一种制备吉美嘧啶的精制方法 |
CN103694165A (zh) * | 2013-11-12 | 2014-04-02 | 江苏正大清江制药有限公司 | 吉美嘧啶无定形固化物及制备方法 |
CN103694165B (zh) * | 2013-11-12 | 2016-05-04 | 江苏正大清江制药有限公司 | 吉美嘧啶无定形固化物及制备方法 |
CN104496972A (zh) * | 2014-12-04 | 2015-04-08 | 浙江大学 | 一种新型替加氟药物共晶及其制备方法 |
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