CN101880873B - Preparation process of 103Pd sealed seed source core - Google Patents
Preparation process of 103Pd sealed seed source core Download PDFInfo
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- CN101880873B CN101880873B CN2010102129682A CN201010212968A CN101880873B CN 101880873 B CN101880873 B CN 101880873B CN 2010102129682 A CN2010102129682 A CN 2010102129682A CN 201010212968 A CN201010212968 A CN 201010212968A CN 101880873 B CN101880873 B CN 101880873B
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Abstract
The invention belongs to the technical field of medical preparations containing radioactive substances, in particular to a preparation process of a palladium [103Pb] sealed seed source core used for medical treatment. The process sequentially comprises the following two steps of: (1) dipping a silver stick into a palladium chloride solution, then taking out and washing by using water; dipping the silver stick into an alkaline ammonia solution of hydrazine, taking out and washing clean by using water; and (2) putting the silver stick in a mixed solution containing palladium chloride, ethylene diamine tetraacetic acid, ammonium hydroxide and hydrazine, and stirring for reacting in the presence of water bath heating to ensure that a layer of 103Pd is uniformly covered on the surface of the silver stick. The preparation process has the advantages of low production cost, no environmental pollution, uniform and dense distribution of the 103Pd on the surface of the silver stick, high utilization ratio of the 103Pd, and the like.
Description
Technical field
The invention belongs to the medicinal preparation technical field that contains radioactive substance, be specifically related to a kind of palladium that is used for therapeutic treatment [
103Pd] preparation technology of sealed seed source source core.
Background technology
Implanting treatment between tissue is with radioactive seed source implantation tumour tissue, utilizes the seed irridiation injury kill tumor cell that radiates of core in a steady stream, reaches the purpose of treatment tumour and alleviation disease.Implant treatment between tissue and be used for the treatment of various noumenal tumours, as prostate cancer, mammary cancer, liver cancer, lung cancer, the cancer of the brain, ovarian cancer etc., obtained, outer radiotherapy is identical even better result of treatment with surgical operation.Simultaneously, this methods of treatment reduces complication reducing operation wound, improves patient's survival rate, and the aspect of improving the quality of living has outstanding advantage.Implant treatment between tissue and be divided into temporary implantation and permanent implanted, temporary implantation is meant radioactive seed source implantation tumour position, takes out after treatment for some time; And permanent implanted being meant no longer taken out radioactive seed source implantation tumour position.Nucleic commonly used has
192Ir,
198Au,
169Yb,
103Pd and
125I etc., wherein
103Pd and
125I is used for permanent implanted.
125The I transformation period is 59.6 days, and the gamma-rays average energy is 28keV, and the predose rate is 9cGy/h, is applicable to treatment good differentiation, the tumour that increasess slowly;
103The Pd transformation period is 16.96 days, and the gamma-rays average energy is 23keV, and the predose rate is 20cGy/h, is applicable to that the treatment differentiation is relatively poor, breeds tumour rapidly.Many documents are right
125I and
103Pd is used for the treatment of the curative effect of treatment of solid tumors such as prostate cancer and has made report extensively and profoundly, and for example Ling et al. uses linear quaternary model to compare on the radiobiological basis of theory
125I and
103The curative effect of Pd, conclusion is: on the basis of clinical application dosage,
125I preponderates in the slower tumour of treatment propagation, and
103Pd breeds rapidly to killing that the tumour cell effect is better than
125I.And for example the animal experiment study of Nag etal. shows:
103The cancer knurl of Pd treatment differentiation difference is more effective.Therefore based on above-mentioned and other some achievements in research,
125I is commonly used to treat early stage tumour, and
103Pd is used for the treatment of the middle and advanced stage tumour more.
Radioactive sealed seed core in a steady stream generally selects silver as carrier, because silver is the mark of X ray, so that estimation with therapeutic dose is accurately located in the seed source during implanted treatment.Generally, the length of silver rod is 3.0mm, and diameter is 0.5mm.Treatment is used
103The Pd sealed seed source is with radioactivity
103Pd is fixed in silver rod, is welded in to make in titanium or the titanium alloy tube.Radioactivity
103The method that Pd is fixed on the silver-colored rod adopts absorption method, electrochemical plating and electroless plating method usually.Though absorption method technology is simple, need be adsorbed with
103The mark that adds X ray such as silver between the microballoon of Pd, and seed source distribution of dose is inhomogeneous.Electrochemical plating complex process, plant and instrument require high, and the production cycle is long, is difficult to carry out large-scale production.And electroless plating method technology, equipment are simple, with short production cycle, are easy to apply.For example U.S. Pat 4702228 discloses a kind of absorption method, and this method contains carrier with microballoons such as aluminum oxide absorption
103Pd in the titanium pipe of then two microballoons being packed into, and places the mark of X ray such as silver-colored rod at two microballoons.This method preparation
103The active zone of Pd sealed seed source is positioned at the two ends in seed source, and microballoon moves in the titanium pipe easily, and the interior distribution of dose of whole seed source region is inhomogeneous and can be unfavorable for clinical application because the displacement of microballoon changes.For example Chinese patent ZL01105243.0 discloses a kind of electroless plating method again, and this method is main solution composition with Palladous chloride, ammonium chloride, ammonia, sodium hypophosphite, regulates pH=10,35 ℃ of following electroless platings 1 hour, makes silver-colored excellent surface coverage one deck
103Pd.As stablizer, but ammonium chloride can reduce speed of reaction to this method when stablizing plating bath with ammonium chloride, and the concentration of required in addition reductive agent sodium hypophosphite is higher, is unfavorable for the stability of plating bath.
Summary of the invention
(1) goal of the invention
The object of the invention is to solve
103Cost height among the existing preparation technology of Pd sealed seed source source core, pollute big,
103The problem that the Pd utilization ratio is low.
(2) technical scheme
For achieving the above object, the invention provides following technical scheme:
A kind of
103The preparation technology of Pd sealed seed source source core comprises following two steps successively:
(1) the silver rod is immersed in the palladium chloride solution, take out water and clean, then the silver rod is immersed in the alkaline ammonia solution of hydrazine, take out water and clean up;
(2) silver-colored rod is placed the mixing solutions of being made up of Palladous chloride, disodium ethylene diamine tetraacetate, ammonium hydroxide, hydrazine, stirring reaction under the condition of water bath heating makes silver rod surface evenly cover one deck
103Pd.
Key is, in the Palladous chloride concentration described in the step (1) is 1～10mmol/L, and silver rod soak time in palladium chloride solution is 1～5min, and the concentration of hydrazine is 1～5mol/L, the concentration of ammonia is 0.1～1mol/L, and silver rod soak time in the alkaline ammonia solution of hydrazine is 1～5min; In the Palladous chloride concentration described in the step (2) is 3～30mmol/L, and disodium ethylene diamine tetraacetate concentration is 0.1～0.3mol/L, and ammonium hydroxide concentration is 2.5～10mol/L, hydrazine concentration is 5～25mmol/L, regulating pH is 8～12, and temperature of reaction is 40～70 ℃, and the reaction times is 30～90min.
Preferred situation, the concentration of Palladous chloride is 2～4mmol/L in step (1), the soak time of silver rod in palladium chloride solution is 2～4 minutes.
The concentration of hydrazine is 1.5～3mol/L in step (1), and the concentration of ammonia is 0.15～0.25mol/L, and the soak time of silver rod in the alkaline ammonia solution of hydrazine is 2～4 minutes.
The concentration of Palladous chloride is 5～15mmol/L in step (2), and disodium ethylene diamine tetraacetate concentration is 0.15～0.25mol/L, and ammonium hydroxide concentration is 5～8mol/L, hydrazine concentration is 10～20mmol/L, pH is 9～11, and temperature of reaction is 45～55 ℃, 50～70 minutes reaction times.
Preferred situation, the concentration of Palladous chloride is 2mmol/L in step (1), the soak time of silver rod in palladium chloride solution is 3 minutes.
The concentration of hydrazine is 2mol/L in step (1), and the concentration of ammonia is 0.2mol/L, and the soak time of silver rod in the alkaline ammonia solution of hydrazine is 3 minutes.
The concentration of Palladous chloride is 10mmol/L in step (2), and disodium ethylene diamine tetraacetate concentration is 0.2mol/L, and ammonium hydroxide concentration is 6.5mol/L, and hydrazine concentration is 15mmol/L, and pH is 11, and temperature of reaction is 50 ℃, 60 minutes reaction times.
In step (2), carry out adding radioactivity before the electroless plating reaction
103Pd solution is by regulating
103The add-on of Pd, control source core activity is between 0.5～2.0mCi.
Described Palladous chloride can replace with the aqueous solution of palladium salt such as the palladium of same concentrations, Palladous nitrate, palladous sulfate, palladium acetylacetonate.
Can adopt a kind of pH value in sodium hydroxide, hydrochloric acid, the acetic acid to regulate to solution.
In this technical scheme, silver-colored rod is activated when helping electroless plating
103Pd is deposited on the surface of silver rod evenly and rapidly; Palladous chloride concentration can not be too little, also should not be too big, hour can not guarantee very much
103Pd influences the homogeneity that single seed source dosage field distributes at the excellent surperficial uniform distribution of silver, and the palladium layer is blocked up when too big, too much absorption
103The ray that Pd emits, and can reduce
103The utilization ratio of Pd; The concentration of hydrazine can not be too little, also should not be too big, and hour can reduce speed of reaction very much and cause
103The utilization ratio of Pd is low excessively, easily causes plating bath to decompose when too big.
(3) beneficial effect
Technical scheme provided by the invention has following advantage:
A) reagent such as the Palladous chloride that this preparation technology adopted, disodium ethylene diamine tetraacetate, ammonium hydroxide, hydrazine all are conventional commercial reagent, and buying is convenient, and low price reduces production cost greatly;
B) in reaction process, there is not irritant gas to produce all the time, do not cause environmental pollution, can guarantee Working environment;
C) silver rod surface
103Pd is evenly distributed, densification,
103Pd utilization ratio height.
Embodiment
The present invention will be further described according to specific embodiment below.
Embodiment one
Present embodiment is most preferred technical scheme, and used reagent is analytical pure.
A kind of
103The preparation technology of Pd sealed seed source source core comprises following two steps successively:
(1) activation of silver rod.(ф 0.5 * 3mm) immersed in the 2mmol/L palladium chloride solution 3 minutes with 100 silver rods, the taking-up water cleans, then silver rod is immersed and take out water after 3 minutes in the alkaline ammonia solution of hydrazine and clean up, the concentration of hydrazine is 2mol/L in the alkaline ammonia solution of described hydrazine, and the concentration of ammonia is 0.2mol/L.
(2)
103The electroless plating of Pd.Configuration 1mL plating bath, Palladous chloride concentration is 10mmol/L in the described plating bath, and disodium ethylene diamine tetraacetate concentration is 0.2mol/L, and ammonium hydroxide concentration is 6.5moll/L, and hydrazine concentration is 15mmol/L, and adds 400mCi's simultaneously
103PdCl
2, regulating pH is 11.The silver-colored rod of preparation in the step (1) is put into plating bath, and stirring reaction is 60 minutes under 50 ℃ of condition of water bath heating, makes surface coverage one deck
103Pd.Take out the silver rod, discard surperficial clear liquid, water cleaning silver rod three times promptly makes
103The source core of Pd sealed seed source, its radioactive activity are 2mCi.Measure the radioactive activity of mixing solutions and supernatant liquor respectively, calculate by following formula
103The adsorption efficiency of Pd:
103Radioactive activity * 100% of the adsorption efficiency of Pd=(radioactive activity of the radioactive activity-supernatant liquor of mixing solutions)/mixing solutions obtains this embodiment's
103The Pd adsorption efficiency is 96%.Go up adsorbed according to the every silver rod that this adsorption efficiency calculated
103The radioactive activity of Pd is greater than 2mCi, but owing to the absorption of silver rod own, the activity of prepared source core only is 2mCi.
Described Palladous chloride can replace with the aqueous solution of palladium salt such as the palladium of same concentrations, Palladous nitrate, palladous sulfate, palladium acetylacetonate.
Embodiment two
Step and method are with embodiment one, and the difference part is: add 100mCi's in the step (2)
103PdCl
2, finally make
103The radioactive activity of the source core of Pd sealed seed source is 0.5mCi.
Embodiment three
Step and method are with embodiment one, the difference part is: be 10mmol/L in the Palladous chloride concentration described in the step (1) wherein, silver rod soak time in palladium chloride solution is 1min, the concentration of hydrazine is 5mol/L, the concentration of ammonia is 1mol/L, silver rod soak time in the alkaline ammonia solution of hydrazine is 1min
103The adsorption efficiency of Pd is 90%.
Embodiment four
Step and method are with embodiment one, the difference part is: be 1mmol/L in the Palladous chloride concentration described in the step (1) wherein, silver rod soak time in palladium chloride solution is 5min, the concentration of hydrazine is 1mol/L, the concentration of ammonia is 0.1mol/L, silver rod soak time in the alkaline ammonia solution of hydrazine is 5min
103The adsorption efficiency of Pd is 92%.
Embodiment five
Step and method are with embodiment one, the difference part is: in the Palladous chloride concentration described in the step (2) is 30mmol/L, disodium ethylene diamine tetraacetate concentration is 0.3mol/L, ammonium hydroxide concentration is 10mol/L, hydrazine concentration is 25mmol/L, and regulating pH is 12, and temperature of reaction is 40 ℃, reaction times is 90min
103The adsorption efficiency of Pd is 91%.
Embodiment six
Step and method are with embodiment one, the difference part is: in the Palladous chloride concentration described in the step (2) is 3mmol/L, disodium ethylene diamine tetraacetate concentration is 0.1mol/L, ammonium hydroxide concentration is 2.5mol/L, hydrazine concentration is 5mmolml/L, and regulating pH is 8, and temperature of reaction is 70 ℃, reaction times is 30min
103The adsorption efficiency of Pd is 93%.
Embodiment seven
Step and method are with embodiment one, the difference part is: be 4mmol/L in the Palladous chloride concentration described in the step (1) wherein, silver rod soak time in palladium chloride solution is 2min, the concentration of hydrazine is 3mol/L, the concentration of ammonia is 0.25mol/L, silver rod soak time in the alkaline ammonia solution of hydrazine is 2min
103The adsorption efficiency of Pd is 94%.
Embodiment eight
Step and method are with embodiment one, the difference part is: be 2mmol/L in the Palladous chloride concentration described in the step (1) wherein, silver rod soak time in palladium chloride solution is 4min, the concentration of hydrazine is 1.5mol/L, the concentration of ammonia is 0.15mol/L, silver rod soak time in the alkaline ammonia solution of hydrazine is 4min
103The adsorption efficiency of Pd is 95%.
Embodiment nine
Step and method are with embodiment one, the difference part is: in the Palladous chloride concentration described in the step (2) is 15mmol/L, disodium ethylene diamine tetraacetate concentration is 0.25mol/L, ammonium hydroxide concentration is 8mol/L, hydrazine concentration is 20mmol/L, and regulating pH is 11, and temperature of reaction is 45 ℃, reaction times is 70min
103The adsorption efficiency of Pd is 94%.
Embodiment ten
Step and method are with embodiment one, the difference part is: in the Palladous chloride concentration described in the step (2) is 5mmol/L, disodium ethylene diamine tetraacetate concentration is 0.15mol/L, ammonium hydroxide concentration is 5mol/L, hydrazine concentration is 10mmolml/L, and regulating pH is 9, and temperature of reaction is 55 ℃, reaction times is 50min
103The adsorption efficiency of Pd is 95%.
Above content be in conjunction with preferred embodiment to specifying that the present invention did, can not assert that the specific embodiment of the present invention only limits to these explanations.Concerning the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deductions and conversion, all should be considered as belonging to protection scope of the present invention.
Claims (10)
1. one kind
103The preparation technology of Pd sealed seed source source core comprises following two steps successively:
(1) the silver rod is immersed in the palladium chloride solution, take out water and clean, then the silver rod is immersed in the alkaline ammonia solution of hydrazine, take out water and clean up;
(2) silver-colored rod is placed the mixing solutions of being made up of Palladous chloride, disodium ethylene diamine tetraacetate, ammonium hydroxide, hydrazine, stirring reaction under the condition of water bath heating makes silver rod surface evenly cover one deck
103Pd;
It is characterized in that: in the Palladous chloride concentration described in the step (1) is 1～10mmol/L, silver rod soak time in palladium chloride solution is 1～5min, the concentration of hydrazine is 1～5mol/L, and the concentration of ammonia is 0.1～1mol/L, and silver rod soak time in the alkaline ammonia solution of hydrazine is 1～5min; In the Palladous chloride concentration described in the step (2) is 3～30mmol/L, and disodium ethylene diamine tetraacetate concentration is 0.1～0.3mol/L, and ammonium hydroxide concentration is 2.5～10mol/L, hydrazine concentration is 5～25mmol/L, regulating pH is 8 ~ 12, and temperature of reaction is 40～70 ℃, and the reaction times is 30～90min.
2. preparation technology according to claim 1 is characterized in that: the concentration of Palladous chloride is 2～4mmol/L in step (1), and the soak time of silver rod in palladium chloride solution is 2～4 minutes.
3. preparation technology according to claim 2 is characterized in that: the concentration of Palladous chloride is 2mmol/L in step (1), and the soak time of silver rod in palladium chloride solution is 3 minutes.
4. preparation technology according to claim 1 is characterized in that: the concentration of hydrazine is 1.5～3mol/L in step (1), and the concentration of ammonia is 0.15～0.25mol/L, and the soak time of silver rod in the alkaline ammonia solution of hydrazine is 2～4 minutes.
5. preparation technology according to claim 4 is characterized in that: the concentration of hydrazine is 2mol/L in step (1), and the concentration of ammonia is 0.2mol/L, and the soak time of silver rod in the alkaline ammonia solution of hydrazine is 3 minutes.
6. preparation technology according to claim 1, it is characterized in that: the concentration of Palladous chloride is 5～15mmol/L in step (2), disodium ethylene diamine tetraacetate concentration is 0.15～0.25mol/L, ammonium hydroxide concentration is 5～8mol/L, hydrazine concentration is 10～20mmol/L, pH is 9 ~ 11, and temperature of reaction is 45 ~ 55 ℃, 50 ~ 70 minutes reaction times.
7. preparation technology according to claim 6, it is characterized in that: the concentration of Palladous chloride is 10mmol/L in step (2), disodium ethylene diamine tetraacetate concentration is 0. 2mol/L, ammonium hydroxide concentration is 6.5mol/L, hydrazine concentration is 15mmol/L, pH is 11, and temperature of reaction is 50 ℃, 60 minutes reaction times.
8. preparation technology according to claim 1 is characterized in that: carry out adding radioactivity before the electroless plating reaction in step (2)
103The solution of Pd.
9. preparation technology according to claim 8 is characterized in that: by regulating
103The add-on of the solution of Pd, control source core activity is between 0.5 ~ 2.0mCi.
10. according to claim 1,2,3,6 or 7 described preparation technologies, it is characterized in that: the aqueous solution of the palladium of described palladium chloride solution usefulness same concentrations, Palladous nitrate, palladous sulfate, palladium acetylacetonate replaces.
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| CN2010102129682A CN101880873B (en) | 2010-06-30 | 2010-06-30 | Preparation process of 103Pd sealed seed source core |
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| CN101880873B true CN101880873B (en) | 2011-12-07 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103415918A (en) * | 2011-03-10 | 2013-11-27 | 富士电机株式会社 | Electronic part and method of manufacturing electronic part |
| CN102735312A (en) * | 2012-06-26 | 2012-10-17 | 成都中核高通同位素股份有限公司 | Low-activity cobalt-60 rodlike material level source and preparation method thereof |
| CN106540282B (en) * | 2015-09-16 | 2019-09-24 | 天津赛德生物制药有限公司 | A kind of preparation method of -103 sealed seed source source core of palladium |
| CN117059296B (en) * | 2023-09-27 | 2024-02-06 | 原子高科股份有限公司 | Preparation method and application of palladium-103 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4702228A (en) * | 1985-01-24 | 1987-10-27 | Theragenics Corporation | X-ray-emitting interstitial implants |
| CN1312117A (en) * | 2001-01-18 | 2001-09-12 | 中国科学院上海原子核研究所 | Pd-103 seed medicine and its prepn |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008124778A2 (en) * | 2007-04-09 | 2008-10-16 | George Fred Harder | Hybrid source containing multi-radionuclides for use in radiation therapy |
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2010
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4702228A (en) * | 1985-01-24 | 1987-10-27 | Theragenics Corporation | X-ray-emitting interstitial implants |
| CN1312117A (en) * | 2001-01-18 | 2001-09-12 | 中国科学院上海原子核研究所 | Pd-103 seed medicine and its prepn |
Non-Patent Citations (1)
| Title |
|---|
| Chunfu Zhang,Yongxian Wang, Haibin Tian, Duanzhi Yin.Preparation of 103Pd seeds PartII."Molecular Plating" of 103Pd onto copper rod.《Journal of Radioanalytical and Nuclear Chemistry》.2002,第253卷(第2期),313–316. |
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