CN101475461A - Iodogen method for preparation of hypericin radioactive iodine marker - Google Patents
Iodogen method for preparation of hypericin radioactive iodine marker Download PDFInfo
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- CN101475461A CN101475461A CNA2009100139988A CN200910013998A CN101475461A CN 101475461 A CN101475461 A CN 101475461A CN A2009100139988 A CNA2009100139988 A CN A2009100139988A CN 200910013998 A CN200910013998 A CN 200910013998A CN 101475461 A CN101475461 A CN 101475461A
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Abstract
The invention discloses an Iodogen method in the process of preparing a hypericin radioiodinated labelled substance, which can effectively improve the labeling rate, and has the advantages of simple preparation method and low cost. The method comprises the following steps: 1) mixing DMSO (Dimethyl sulfoxide) solution of the hypericin with a radioiodinated aqueous solution with pH value of between 6.5 and 7.5, and taking no hypericin precipitation as the condition of meeting requirement after being mixed; and adding the radioiodinated aqueous solution according to the required radioactivity amount during mixing; 2) adding an oxidant 1,3,4,6-Tetrachloro-3alpha,6alpha-Diphenylglycouril(trade-name: Iodogen) into the mixed solution, wherein the dosage of the oxidant meets the requirement of an excessive reaction according to the radioactive iodine; 3) reacting the prepared mixed solution at room temperature for 2 to 10 minutes; and 4) sampling and subjecting the reacted solution to measurement of the labeling rate.
Description
Technical field
The present invention relates to the Iodogen method in a kind of hypericin radioiodide preparation process.
Background technology
Hypericin (hypericin) is a kind of plant milk extract, and existing now artificial synthesis is used to some extent in treatment dysthymia disorders and aspect such as antiviral at present.The hypericin radioiodide is the radioiodide that forms with the hydrogen on the radioiodine replacement hypericin, might be used for tumour, the diagnosis of diseases such as myocardial infarction and treatment (external existing relevant patent).In the hypericin radioiodide preparation process, relate to the use of oxygenant.In of the report of existing use Peracetic Acid as oxygenant, mark rate has only about 60%, and (document sees reference: Sang Wook Kim, Jeong Hoon Park, Seung DaeYang, Min Goo Hur, Chang Woon Choi, and Kook Hyun Yu, Bull.Korean Chem.Soc.2008, Vol.29, No.102023), must be before marker uses through purifying.Cause preparation process very loaded down with trivial details thus, and the cycle is long, expense height, mark rate also can't be satisfactory.
Summary of the invention
Purpose of the present invention is exactly provide a kind of and can effectively improve mark rate, and the preparation method to be easy in order to address the above problem, the Iodogen method in the lower hypericin radioiodide preparation process of expense.
For achieving the above object, the present invention adopts following technical scheme:
Iodogen method in a kind of hypericin radioiodide preparation process,
1) is the radioiodine aqueous solution of 6.5-7.5 with hypericin DMSO (Dimethyl sulfoxide) solution and pH value, mixes the back and separate out to meeting the demands with no hypericin; The amount of the hypericin DMSO solution and the radioiodine aqueous solution all adds by the required amount of preparation marker.(because the high specific activity of this marker is 2.5*10
10MCi/mg, and can not use so big specific activity in the practical application, so hypericin is always excessive in labeling process.)
2) in mixed solution, add the oxygenant 1,3,4 that commodity are called Iodogen, 6-Tetrachloro-3 α, 6 α-Diphenylglycouril, the excessive response requirement is determined and satisfied to its consumption according to radioiodine;
3) mixed solution for preparing at room temperature reacted 2-10 minute;
4) sampling is carried out mark rate and is measured and to get final product.
In the described step 1), radioiodine is iodine-131 or iodo-123 or iodo-124 or iodine-125.
Described step 2) in, the oxygenant Iodogen of adding adopts any one of following two kinds of forms, and wherein a kind of is freshly prepared Iodogen DMSO solution; Another kind of is mixed solution to be added the Iodogen for preparing be coated with in the pipe; This dual mode all should satisfy the oxygenant Iodogen with q.s.
When described radioiodine was iodine-131, the consumption of Iodogen was that the used Iodogen amount of every millicurie iodine is no less than 20 micrograms.
When described radioiodine was iodo-123, the consumption of Iodogen was that the used Iodogen amount of every millicurie iodine is no less than 1.3 micrograms.
When described radioiodine was iodo-124, the consumption of Iodogen was that the used Iodogen amount of every millicurie iodine is no less than 10 micrograms.
When described radioiodine was iodine-125, the consumption of Iodogen was that the used Iodogen amount of every millicurie iodine is no less than 140 micrograms.
Described Iodogen is coated with the preparation of pipe: compound concentration is a 1mg/ml Iodogen/ dichloromethane solution, and solution is added in glass or the plastic test tube quantitatively, with nitrogen methylene dichloride is dried up, and promptly makes Iodogen and is coated with pipe, is coated with pipe and preserves in 4 degrees centigrade of refrigerators.
The freshly prepared Iodogen DMSO strength of solution of described adding is 2mg/ml.
The present invention has proposed to adopt the hypericin labelling method of Iodogen as oxygenant first, layoutprocedure to radioactive iodine concentration and hypericin liquid on concentration without limits, can be configured respectively according to the mark needs, but should guarantee that radioactive iodine is neutral (as not being neutral, then should be adjusted into neutrality earlier can use), two kinds of solution are also unqualified on the blended ratio simultaneously, but must guarantee that mixed solution does not have hypericin to separate out the requirement that can satisfy use.Then oxygenant Iodogen is joined in the mixed solution, wherein the consumption of oxygenant Iodogen is relevant with radioiodine kind and the consumption selected for use, and makes oxygenant Iodogen adopt excessive response.The radioactive iodine consumption then can add just according to required radioactivity amount in conjunction with existing general knowledge, and this belongs to the known technology scope, and the present invention no longer gives unnecessary details it.
The invention has the beneficial effects as follows: the mark rate height, can reach more than 99%, preparation process is simple simultaneously, and the time is short, and cost is low.
Description of drawings:
Fig. 1 is an Iodogen method radioiodination hypericin reaction formula synoptic diagram.
Embodiment
The invention will be further described below in conjunction with accompanying drawing and embodiment.
Iodogen method in a kind of hypericin radioiodide preparation process,
1) is the radioiodine aqueous solution of 6.5-7.5 with hypericin DMSO (Dimethyl sulfoxide) solution and pH value, mixes the back and separate out to meeting the demands with no hypericin; The radioiodine aqueous solution adds by required radioactivity amount during mixing;
2) in mixed solution, add the oxygenant 1,3,4 that commodity are called Iodogen, 6-Tetrachloro-3 α, 6 α-Diphenylglycouril, the excessive response requirement is determined and satisfied to its consumption according to radioiodine;
3) mixed solution for preparing at room temperature reacted 2-10 minute;
4) sampling is carried out mark rate and is measured and to get final product.
In the described step 1), radioiodine is iodine-131 or iodo-123 or iodo-124 or iodine-125.
Described step 2) in, the oxygenant Iodogen of adding adopts any one of following two kinds of forms, and wherein a kind of is freshly prepared Iodogen DMSO solution; Another kind of is mixed solution to be added the Iodogen for preparing be coated with in the pipe; This dual mode all should satisfy the requirement of oxygenant Iodogen excessive response.
When described radioiodine was iodine-131, the consumption of Iodogen was that the used Iodogen amount of every millicurie iodine is no less than 20 micrograms, as 25 micrograms or 30 micrograms or 40 micrograms.
When described radioiodine was iodo-123, the consumption of Iodogen was that the used Iodogen amount of every millicurie iodine is no less than 1.3 micrograms, as 2 micrograms or 5 micrograms or 8 micrograms.
When described radioiodine was iodo-124, the consumption of Iodogen was that the used Iodogen amount of every millicurie iodine is no less than 10 micrograms, as 15 micrograms or 20 micrograms or 40 micrograms.
When described radioiodine was iodine-125, the consumption of Iodogen was that the used Iodogen amount of every millicurie iodine is no less than 140 micrograms, as 150 micrograms or 180 micrograms or 200 micrograms.
Described Iodogen is coated with the preparation of pipe: compound concentration is a 1mg/ml Iodogen/ dichloromethane solution, and solution is added in glass or the plastic test tube quantitatively, with nitrogen methylene dichloride is dried up, and promptly makes Iodogen and is coated with pipe, is coated with pipe and preserves in 4 degrees centigrade of refrigerators.
The freshly prepared Iodogen DMSO strength of solution of described adding is 2mg/ml.
Embodiment 1:
The mark route that this patent proposes, the oxygenant of use is 1,3,4,6-Tetrachloro-3 α, (trade(brand)name: Iodogen), mark rate can reach more than 99% 6 α-Diphenylglycouril, and reaction solution can directly use.
Concrete path label is as follows:
A：
1. in iodine-131 solution (50 μ l, 12mCi are dissolved in the 0.1N NaOH aqueous solution), add acidic solution (0.1N HCl, 50 μ l), add hypericin DMSO solution (2mg/ml, 400 μ l) again.
2. add freshly prepared Iodogen DMSO (2mg/ml, 200 μ l) solution in the mixed solution.
3. reacted 10 minutes under the room temperature.
4. sampling is carried out ply of paper and is analysed (No. 1 filter paper of Xinhua, 0.1N HCl is a developping agent, after the expansion, the mark hypericin is positioned at initial point, free radioactivity iodine is positioned at the forward position).
5. the mark rate of measuring with gamma counter is 99.4%.
B：
1. in iodine-131 solution (10 μ l, 1mCi, the aqueous solution), add hypericin DMSO solution (1mg/ml, 60 μ l).
2. mixed solution is moved into Iodogen and be coated with pipe (containing Iodogen 20ug)
3. reacted 10 minutes under the room temperature.
4. sampling is carried out ply of paper and is analysed (No. 1 filter paper of Xinhua, 0.1N HCl is a developping agent, after the expansion, the mark hypericin is positioned at initial point, free radioactivity iodine is positioned at the forward position).
5. the mark rate of measuring with gamma counter is 99.3%.
This labeling process has carried out tens times, and average mark rate is 99.4 ± 0.4%, n=29.
Iodogen is coated with the preparation of pipe: preparation 1mg/ml Iodogen/ dichloromethane solution, solution is added in glass or the plastic test tube quantitatively, and with nitrogen methylene dichloride is dried up, promptly make Iodogen and be coated with pipe.Be coated with pipe and preserve in 4 degree refrigerators, can standby for a long time (at least one year).
Because isotopic each nucleic has identical chemical property, the labeling process of iodine-131 and the mark rate of acquisition be applicable to iodo-123, iodo-124, iodine-125.
Claims (9)
1. the lodogen method in the hypericin radioiodide preparation process is characterized in that,
1) the radioiodine aqueous solution that the DMSO solution and the pH value of hypericin is 6.5-7.5 is mixed the back and is separated out to meeting the demands with no hypericin; The amount of the hypericin DMSO solution and the radioiodine aqueous solution all adds by the required amount of preparation marker;
2) adding trade name in the solution that mixes is the oxygenant 1,3,4 of lodogen, 6-Tetrachloro-3 α, and 6 α-Diphenylglycouril, the excessive response requirement is determined and satisfied to its consumption according to radioiodine;
3) mixed solution for preparing at room temperature reacted 2-10 minute;
4) sampling is carried out mark rate and is measured and to get final product.
2. the lodogen method in the hypericin radioiodide preparation process as claimed in claim 1 is characterized in that, in the described step 1), radioiodine is iodine-131 or iodo-123 or iodo-124 or iodine-125.
3. the lodogen method in the hypericin radioiodide preparation process as claimed in claim 1, it is characterized in that, described step 2) in, the oxygenant lodogen of adding adopts any one of following two kinds of forms, and wherein a kind of is freshly prepared Iodogen DMSO solution; Another kind of is mixed solution to be added the lodogen for preparing be coated with in the pipe; This dual mode all should satisfy and has excessive oxygenant lodogen.
4. as the lodogen method in claim 1 or the 2 or 3 described hypericin radioiodide preparation process, it is characterized in that when described radioiodine was iodine-131, the consumption of lodogen was that the used lodogen amount of every millicurie iodine is no less than 20 micrograms.
5. as the lodogen method in claim 1 or the 2 or 3 described hypericin radioiodide preparation process, it is characterized in that when described radioiodine was iodo-123, the consumption of lodogen was that the used lodogen amount of every millicurie iodine is no less than 1.3 micrograms.
6. as the lodogen method in claim 1 or the 2 or 3 described hypericin radioiodide preparation process, it is characterized in that when described radioiodine was iodo-124, the consumption of lodogen was that the used lodogen amount of every millicurie iodine is no less than 10 micrograms.
7. as the lodogen method in claim 1 or the 2 or 3 described hypericin radioiodide preparation process, it is characterized in that when described radioiodine was iodine-125, the consumption of lodogen was that the used lodogen amount of every millicurie iodine is no less than 140 micrograms.
8. the lodogen method in the hypericin radioiodide preparation process as claimed in claim 3, it is characterized in that, described lodogen is coated with the preparation of pipe: compound concentration is a 1mg/ml lodogen/ dichloromethane solution, solution is added in glass or the plastic test tube quantitatively, with nitrogen methylene dichloride is dried up, promptly make lodogen and be coated with pipe, be coated with pipe and preserve in 4 degrees centigrade of refrigerators.
9. the lodogen method in the hypericin radioiodide preparation process as claimed in claim 3 is characterized in that, the freshly prepared lodogen DMSO strength of solution of described adding is 2mg/ml.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102488910A (en) * | 2011-12-29 | 2012-06-13 | 江苏省中医药研究院 | Application of radioisotope-marked sunshine anthrone compound in preparing anti-tumor medicine |
| CN107308455A (en) * | 2017-06-27 | 2017-11-03 | 南京成至诚医药科技有限公司 | Application of the cyclodextrin in radioidination Hypericum Chinense class pharmaceutical preparation is prepared |
| CN114181155A (en) * | 2021-12-21 | 2022-03-15 | 上海朝晖药业有限公司 | Iodine-enzalutamide and preparation method and application thereof |
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2009
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102488910A (en) * | 2011-12-29 | 2012-06-13 | 江苏省中医药研究院 | Application of radioisotope-marked sunshine anthrone compound in preparing anti-tumor medicine |
| CN102488910B (en) * | 2011-12-29 | 2013-10-02 | 江苏省中医药研究院 | Application of radioisotope-marked sunshine anthrone compound in preparing anti-tumor medicine |
| CN107308455A (en) * | 2017-06-27 | 2017-11-03 | 南京成至诚医药科技有限公司 | Application of the cyclodextrin in radioidination Hypericum Chinense class pharmaceutical preparation is prepared |
| CN114181155A (en) * | 2021-12-21 | 2022-03-15 | 上海朝晖药业有限公司 | Iodine-enzalutamide and preparation method and application thereof |
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Owner name: CHANGZHOU YICHENG PHARMACEUTICAL TECHNOLOGY CO., L Free format text: FORMER OWNER: INST. OF RADIO MEDICINE, SHANDONG ACADEMY OF MEDICAL SCIENCE Effective date: 20130311 |
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Free format text: CORRECT: ADDRESS; FROM: 250062 JINAN, SHANDONG PROVINCE TO: 213022 CHANGZHOU, JIANGSU PROVINCE |
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Effective date of registration: 20130311 Address after: 213022 No. 18, Huashan Road, Xinbei District, Jiangsu, Changzhou 3-502 Patentee after: Changzhou to Pharmaceutical Technology Co., Ltd. Address before: 250062, No. ten, No. 89, Lixia District, Ji'nan City, Shandong Province Patentee before: Inst. of Radio Medicine, Shandong Academy of Medical Science |
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Effective date of registration: 20160113 Address after: Cheng Wei Road Nanjing city Jiangsu province 210000 Xianlin University No. 9 Patentee after: Nanjing Zhicheng medical science and Technology Co Ltd Address before: 213022 No. 18, Huashan Road, Xinbei District, Jiangsu, Changzhou 3-502 Patentee before: Changzhou to Pharmaceutical Technology Co., Ltd. |