CN1679811A - 一种丹参提取物、其制备方法、药物制剂及检测方法 - Google Patents
一种丹参提取物、其制备方法、药物制剂及检测方法 Download PDFInfo
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- CN1679811A CN1679811A CN 200510037786 CN200510037786A CN1679811A CN 1679811 A CN1679811 A CN 1679811A CN 200510037786 CN200510037786 CN 200510037786 CN 200510037786 A CN200510037786 A CN 200510037786A CN 1679811 A CN1679811 A CN 1679811A
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- salvianolic acid
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Abstract
Description
工艺项目 | 老工艺 | 已知专利工艺 | 新发明工艺 |
批生产周期(天) | 25-30 | / | 2 |
批冷藏期(天) | 14 | / | 0 |
批耗用乙醇比例 | 5 | 3 | 1 |
批浓缩时间比例 | 5 | / | 1 |
批电量消耗比例 | 5 | / | 1 |
丹参素得量(mg/16g药材) | / | / | >80 |
丹参素收率(以药材计,%) | 0.2-0.3 | 0.02 | >0.5 |
丹参素占总固体物的量(%) | 5-10 | / | 28-38 |
原儿茶醛得量(mg/16g药材) | / | / | >25 |
原儿茶醛收率(以药材计,%) | / | 0.005 | >0.15 |
原儿茶醛占总固体物的量(%) | / | / | 9-18 |
丹酚酸B得量(mg/16g药材) | / | / | >80 |
丹酚酸B收率(以药材计,%) | / | 0.56 | >0.5 |
丹酚酸B占总固体物的量(%) | / | / | 29-38 |
总有效部位得量(mg/16g药材) | / | 93 | >210 |
总有效部位收率(%) | 0.25-0.35 | 0.58 | >1.3 |
丹灵总量占总固体物的量(%) | / | 34.5 | >82 |
成品的色度 | 深 | / | 浅 |
稳定性存放时间(年) | <2 | / | 2 |
每1万瓶节省成本 | / | / | 8000元 |
成分 | 投料量(g) |
丹灵甘露醇 | 2500ml30.0 |
成分 | 投料量 |
丹灵氯化钠 | 2500ml2250g |
成分 | 投料量 |
丹灵葡萄糖 | 2500ml12500g |
成分 | 投料量(g) |
丹灵粉聚乙二醇6000 | 1080 |
批号 | 02 | 03 | 04 | 05 | 06 | 分子量 | 成分名称 | 平均相对保留时间 |
1 | 9.212/9.212(1) | 9.237/9.237(1) | 9.223/9.223(1) | 9.204/9.204(1) | 0.797/0.797(1) | 198 | 丹参素 | 1.00 |
2 | 12.167/9.212(1.321) | / | / | / | 358 | 原紫草酸 | 1.32 | |
3 | 12.557/9.212(1.363) | / | / | / | 358 | 原紫草酸 | 1.36 | |
4 | 13.649/9.212(1.482) | 13.616/9.237(1.474) | 13.603/9.223(1.475) | 13.594/9.204(1.477) | 12.957/8.797(1.472) | 138 | 原儿茶醛 | 1.48 |
5 | 18.089/9.212(1.964) | 18.014/9.237(1.950) | 17.989/9.223(1.950) | 18.009/9.204(1.957) | 17.502/8.797(1.989) | 180 | 咖啡酸 | 1.96 |
6 | 21.249/9.212 | 20.648/9.237 | 20.616/9.223 | 20.658/9.204 | 20.265/8.797 | 538 | 紫草酸 | 2.26 |
(2.307) | (2.235) | (2.235) | (2.244) | (2.304) | ||||
7 | 21.749/9.212(2.361) | 21.229/9.237(2.298) | 21.194/9.223(2.298) | 21.224/9.204(2.306) | 20.834/8.797(2.426) | 538 | 紫草酸 | 2.34 |
8 | 22.351/9.212(2.426) | 22.330/9.237(2.417) | 22.294/9.223(2.417) | 22.329/9.204(2.426) | 21.941/8.797(2.494) | 538 | 紫草酸 | 2.44 |
9 | 24.172/9.212(2.624) | 24.137/9.237(2.613) | 24.092/9.223(2.612) | 24.135/9.204(2.622) | 23.718/8.797(2.696) | 538 | 紫草酸 | 2.63 |
10 | 25.251/9.212(2.741) | 25.246/9.237(2.733) | 25.196/9.223(2.732) | 25.237/9.204(2.742) | 24.281/8.797(2.760) | 718 | 丹酚酸B | 2.74 |
11 | 25.748/9.212(2.795) | 25.771/9.237(2.790) | 25.717/9.223(2.788) | 25.752/9.204(2.798) | 24.842/8.797(2.824) | 718 | 丹酚酸B | 2.80 |
12 | 26.918/9.212(2.922) | 26.921/9.237(2.915) | 26.848/9.223(2.911) | 26.883/9.204(2.921) | 26.422/8.797(3.004) | 418 | 丹酚酸D | 2.93 |
13 | 27.899/9.212(3.029) | 27.938/9.237(3.025) | 27.879/9.223(3.023) | 27.915/9.204(3.033) | 26.422/8.797(3.004) | 718 | 丹酚酸B | 3.02 |
14 | 28.293/9.212(3.071) | 27.938/9.237(3.025) | 28.214/9.223(3.059) | 28.248/9.204(3.069) | 27.468/8.797(3.122) | 360 | 迷迭香酸 | 3.07 |
15 | 30.040/9.212(3.261) | / | / | / | 27.733/8.797(3.153) | 494 | 丹酚酸A | 3.21 |
16 | 30.243/9.212(3.283) | 30.168/9.223(3.271) | 30.168/9.223(3.271) | 30.211/9.204(3.282) | 28.621/8.797(3.253) | 718 | 丹酚酸B | 3.27 |
17 | 30.961/9.212(3.361) | 30.938/9.237(3.349) | 30.884/9.223(3.349) | 30.926/9.204(3.360) | 29.878/8.797(3.396) | 494 | 丹酚酸A | 3.36 |
18 | 34.996/9.212(3.799) | 35.005/9.237(3.790) | 296 | 丹参醇B或丹参醌VI | 3.79 | |||
19 | 36.544/9.212(3.967) | / | / | / | 36.136/8.797(4.108) | 492 | 丹酚酸C | 4.04 |
浓度(ug/ml) | 184.15 | 294.64 | 368.3 | 441.96 | 552.45 |
面积(S) | 4538.634 | 7206.369 | 9052.418 | 10799.16 | 13242.01 |
S=23.736c+225.92 r=0.9997 |
序号 | 1 | 2 | 3 | 4 | 5 | RSD(%) |
面积(S) | 3271.68 | 3278.42 | 3296.074 | 3306.948 | 3278.365 | 0.45 |
时间(h) | 0 | 2h | 4h | 8h | RSD(%) |
总含量(mg/ml) | 494.42 | 504.41 | 508.21 | 495.12 | 1.37 |
序号 | 样品含量(mg) | 对照品加入量(mg) | 测得总量(mg) | 对照品测得量(mg) | 回收率(%) |
1 | 50.10 | 51.41 | 101.59 | 51.49 | 100.16 |
2 | 50.10 | 51.41 | 101.67 | 51.57 | 100.31 |
3 | 50.10 | 51.41 | 101.67 | 51.57 | 100.31 |
4 | 50.10 | 51.41 | 101.44 | 51.34 | 99.86 |
5 | 50.10 | 51.41 | 101.70 | 51.60 | 100.37 |
X±SD=100.20%±0.21 RSD=0.21% |
序号 | 样品含量(mg) | 对照品加入量(mg) | 测得总量(mg) | 对照品测得量(mg) | 回收率(%) |
1 | 4.22 | 4.44 | 8.65 | 4.43 | 99.77 |
2 | 4.22 | 4.44 | 8.66 | 4.44 | 100.0 |
3 | 4.22 | 4.44 | 8.68 | 4.46 | 100.45 |
4 | 4.22 | 4.44 | 8.66 | 4.44 | 100.0 |
5 | 4.22 | 4.44 | 8.67 | 4.45 | 100.23 |
X±SD=100.09%±0.26 RSD=0.26% |
序号 | 样品含量(mg) | 对照品加入量(mg) | 测得总量(mg) | 对照品测得量(mg) | 回收率(%) |
1 | 39.20 | 36.05 | 75.01 | 35.81 | 99.33 |
2 | 39.20 | 36.05 | 74.92 | 35.72 | 99.08 |
3 | 39.20 | 36.05 | 74.95 | 35.75 | 99.17 |
4 | 39.20 | 36.05 | 74.94 | 35.74 | 99.14 |
5 | 39.20 | 36.05 | 74.94 | 35.74 | 99.14 |
X±SD=99.17%±0.09 RSD=0.09% |
序号 | 1 | 2 | 3 | 4 | 5 | 6 | RSD(%) |
总含量(mg/ml) | 538.43 | 530.29 | 496.67 | 500.49 | 520.58 | 514.87 | 3.17 |
序号 | 相对保留时间 | 与相对保留时间相应的各成分名称 |
1 | 1.00 | 丹参素(Danshensu) |
2 | 约1.32 | 原紫草酸(Prolithospermic acid) |
3 | 约1.36 | 原紫草酸(Prolithospermic acid) |
4 | 约1.48 | 原儿茶醛(Protocatechualdehyde) |
5 | 约1.96 | 咖啡酸(Caffeic acid) |
6 | 约2.26 | 紫草酸(Lithospermic acid) |
7 | 约2.34 | 紫草酸(Lithospermic acid) |
8 | 约2.44 | 紫草酸(Lithospermic acid) |
9 | 约2.63 | 紫草酸(Lithospermic acid) |
10 | 约2.74 | 丹酚酸B(Salvianolic acid B) |
11 | 约2.80 | 丹酚酸B(Salvianolic acid B) |
12 | 约2.93 | 丹酚酸D(Salvianolic acid D) |
13 | 约3.02 | 丹酚酸B(Salvianolic acid B) |
14 | 约3.06 | 迷迭香酸(Rosmerinic acid) |
15 | 约3.21 | 丹酚酸A(Salvianolic acid A) |
16 | 约3.27 | 丹酚酸B(Salvianolic acid B) |
17 | 约3.36 | 丹酚酸A(Salvianolic acid A) |
18 | 约3.79 | 丹参醇B(Tanshinol B)或丹参醌VI(Tanshinone VI) |
19 | 约4.04 | 丹酚酸C(Salvianolic acid C) |
批号 | 030318 | 030319 | 030320 |
丹灵(有效部位)总含量(mg/ml) | 186.045 | 223.975 | 236.045 |
丹参素(mg/ml) | 47.6 | 49.13 | 52.785 |
原儿茶醛(mg/ml) | 5.35 | 6.675 | 7.805 |
丹灵(有效部位)总含量/总固体量(%) | 93.02 | 82.65 | 84.91 |
Claims (10)
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101012163B (zh) * | 2006-11-03 | 2010-05-12 | 上海朗萨医药科技有限公司 | 一种高纯度丹参素的制备方法 |
CN1951892B (zh) * | 2005-10-21 | 2010-10-27 | 山东绿叶天然药物研究开发有限公司 | 一种原儿茶醛的制备方法 |
CN101538258B (zh) * | 2009-03-04 | 2012-12-19 | 沈阳药科大学 | 丹参中的化合物、其衍生物及其制备方法和医药用途 |
CN106860513A (zh) * | 2016-12-31 | 2017-06-20 | 上海华源安徽锦辉制药有限公司 | 一种丹参滴注液及其生产过程质量控制方法 |
CN108339008A (zh) * | 2017-01-25 | 2018-07-31 | 邢为藩 | 一种丹酚制剂在抗脑缺血再灌注损伤药物中的应用 |
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CN1264533C (zh) * | 2002-06-07 | 2006-07-19 | 上海祥鹤制药厂 | 一种复方丹参胶囊及制备方法 |
CN1470255A (zh) * | 2002-07-22 | 2004-01-28 | 王智民 | 自丹参三七中提取的制备物及其复方制备方法和医疗用途 |
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Cited By (5)
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CN1951892B (zh) * | 2005-10-21 | 2010-10-27 | 山东绿叶天然药物研究开发有限公司 | 一种原儿茶醛的制备方法 |
CN101012163B (zh) * | 2006-11-03 | 2010-05-12 | 上海朗萨医药科技有限公司 | 一种高纯度丹参素的制备方法 |
CN101538258B (zh) * | 2009-03-04 | 2012-12-19 | 沈阳药科大学 | 丹参中的化合物、其衍生物及其制备方法和医药用途 |
CN106860513A (zh) * | 2016-12-31 | 2017-06-20 | 上海华源安徽锦辉制药有限公司 | 一种丹参滴注液及其生产过程质量控制方法 |
CN108339008A (zh) * | 2017-01-25 | 2018-07-31 | 邢为藩 | 一种丹酚制剂在抗脑缺血再灌注损伤药物中的应用 |
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