CN101797392B - Palladium-103 and io-125 compound sealed seed source, source core and source core preparation method - Google Patents
Palladium-103 and io-125 compound sealed seed source, source core and source core preparation method Download PDFInfo
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- CN101797392B CN101797392B CN2010101047007A CN201010104700A CN101797392B CN 101797392 B CN101797392 B CN 101797392B CN 2010101047007 A CN2010101047007 A CN 2010101047007A CN 201010104700 A CN201010104700 A CN 201010104700A CN 101797392 B CN101797392 B CN 101797392B
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Abstract
The invention belongs to the technical field of medical preparations containing radioactive substances, in particular to a palladium-103 and io-125 compound sealed seed source, a source core and a source core preparation method. A palladium-103 and io-125 compound film covers on a carrier to form the source core, and the palladium-103 and io-125 compound sealed seed source is prepared in a way that the source core is welded and sealed in a titanium pipe or titanium alloy pipe. The source core preparation method of the palladium-103 and io-125 compound sealed seed source comprises the steps of: 1, inoculating a nano palladium seed crystal: dipping a carrier bar into a chloroform solution of palladium diacetate, and then dipping into an alkaline ammonia solution of hydrazine; 2, carrying out chemical plating on palladium-103 and silver: putting the carrier bar into a mixed solution of palladium chloride, silver nitrate, ethylene diamine tetraacetic acid, ammonium hydroxide and hydrazine to enable the surface of a carrier to be uniformly coated with a layer of palladium-103 and silver; and 3, carrying out chemical absorption of iodine-125: putting the carrier bar into a mixed solution of sodium bromide or potassium bromide, sodium iodide or potassium iodide, sodium hydroxide or potassium hydroxide, and potassium ferricyanide.
Description
Technical field
The invention belongs to the medicinal preparation technical field that contains radioactive substance, be specifically related to a kind of palladium-103 and iodine-125 compound seal seed source, source core and source core method for preparing.
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 tumor and alleviation disease.Implant treatment between tissue and be used for the treatment of various entity tumors, like carcinoma of prostate, breast carcinoma, hepatocarcinoma, pulmonary carcinoma, the brain cancer, ovarian cancer etc., obtained, outer radiotherapy is identical even better therapeutic effect with surgical operation.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 a period of time; And permanent implanted being meant no longer taken out radioactive seed source implantation tumour position.Implant the common employing of treatment between permanent tissue and be prepared into the seed source than short and the lower radionuclide of ray energy, like iodine-125 seed source and palladium-103 seed source by the half-life.
The iodine-125 half-life 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 tumor that increasess slowly; Palladium-103 half-life 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 tumor rapidly.Many documents have been made report extensively and profoundly to the curative effect that iodine-125 and palladium-103 are used to treat treatment of solid tumors such as carcinoma of prostate; For example Ling et al. uses linear quaternary model on the radiobiological basis of theory, to compare the curative effect of iodine-125 and palladium-103; Conclusion is: on the basis of clinical practice dosage; Iodine-125 is preponderated in the slower tumor of treatment propagation, and palladium-103 pair kills and to breed rapidly that the tumor cell effect is better than iodine-125.And for example the animal experiment study of Nag et al. shows: the carcinoma of palladium-103 treatment poor differentiation is more effective.Therefore based on above-mentioned and other some achievements in research, iodine-125 is commonly used to treat early stage tumor, and is used to treat the middle and advanced stage tumor palladium-103 more.
Treatment is that radioactivity palladium-103 is fixed in silver is excellent with palladium-103 sealed seed source, is welded in to process in titanium or the titanium alloy tube.The method that the radioactivity iodine-125 is fixed on the silver-colored rod adopts galvanoplastic and chemiadsorption usually.Galvanoplastic require shortcomings such as high, production cycle length owing to complex process, instrument and equipment, be difficult to apply.Comparatively speaking, chemiadsorption technology, equipment are simple, with short production cycle, are easy in large-scale production, use.For example United States Patent (USP) 4323055 discloses a kind of chemiadsorption, and this method is that the silver rod was handled 1.5 hours with the hydrochloric acid mixed solution of sodium chlorite and 6mol/L, makes silver-colored excellent surface oxidation, chlorination, obtains the silver rod of surface coverage silver nitride precipitation; Again with itself and iodine [
125I] change sodium solution and under the condition of pH=10, carried out ion-exchange reactions 18 hours, make silver nitride precipitation be converted into iodine [
125I] change silver deposition.In this method, sodium chlorite is not conventional reagent, is difficult to buying on the market; And produce the chlorine that penetrating odor is arranged in a large number in the course of reaction, environment is polluted.
Treatment is that radioactivity palladium-103 is fixed in silver is excellent with palladium-103 sealed seed source, is welded in to process in titanium or the titanium alloy tube.The method that radioactivity palladium-103 is fixed on the silver-colored rod adopts galvanoplastic and electroless plating method usually.Galvanoplastic complex process, instrument and equipment 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 Chinese patent ZL01105243.0 discloses a kind of electroless plating method, and this method is to be main solution composition with Palladous chloride., ammonium chloride, ammonia, sodium hypophosphite, regulates pH=10,35 ℃ of following chemical platings 1 hour, makes silver-colored excellent surface coverage one deck palladium-103.The silver-colored rod of the surface coverage palladium-103 that obtains in this method is difficult to adsorb iodine-125 in the above, can only prepare palladium-103 seed source.
Mostly present research is to treat single nucleic seed source implantation tumour of planting.-103 two kinds of radioactive seed sources of iodine-125 and palladium can mixing application.The half-life of palladium-103 is 16.96 days, and the dosage of release 50% has only 8.5 days, becomes " the line army " that attack tumor cell; 59.6 days iodine-125 half-life, the dosage of release 50% needs 30 days, just in time becomes palladium-103 " second echelon " afterwards.This imagination based on radiobiological effect also because palladium-103 be applicable to poor differentiation, the fast tumor cell of propagation, and iodine-125 is applicable to good differentiation, divides slower tumor cell, both share and can more comprehensively attack tumor cell.For example research such as Chen is thought, if in the iodine-125 seed source plantation treatment of using clinical survival dose, mix and implant palladium-103 seed source, will increase the lethality to tumor cell; On the other hand; If when using clinical survival dose plantation palladium-103 seed source treatment tumor; Mix the iodine-125 seed source of implanting; The main position of dose distribution will produce radiobiology so-called " cold spot " (reparation that is this scope inner cell survival or the inferior cell that causes death increases) in iodine-125 seed source so, and for the tumor rapidly of growing, " cold spot " effect is particularly evident.But; On carrier, plate palladium-103 simultaneously and have certain difficulty with iodine-125; If while depositing Pd-103 and iodine-125 on carrier, because two kinds of nucleic chemical property are widely different, the deposition of palladium-103 need adopt Reducing agent; And the deposition of iodine-125 needs oxidant, and the two can not be present in in a kind of solution simultaneously; If on carrier, plate earlier palladium-103, because palladic chemical property is stable, deposition iodine-125 above being difficult in; If plate iodine-125 earlier, there is NH in iodine-125 with the form deposition of AgI during owing to chemical palladium-plating
4OH can cause a large amount of losses of AgI.Based on above reason, the research of having reported at present only limits to palladium-103 seed source and iodine-125 seed source implantation tumour tissue respectively, does not have still that palladium-103 and iodine-125 are compound to be the seed source of one.
Summary of the invention
(1) goal of the invention
The object of the invention is to provide a kind of palladium-103 and iodine-125 compound seal seed source, source core and source core method for preparing.
(2) technical scheme
For realizing above-mentioned purpose, the present invention provides following technical scheme:
The source core in a kind of palladium-103 and iodine-125 compound seal seed source; With can as the metal of X ray label or nonmetal be carrier; On this carrier, cover one deck radiosiotope thin film, key is: said radiosiotope thin film is the laminated film of palladium-103 and iodine-125.Said metallic carrier is processed by wherein a kind of of silver, copper, nickel, palladium, gold or the alloy that contains this metal, and said non-metal carrier is processed by resin, plastics.Said support shapes can be bar-shaped or round shaped grain shape.Said support rod specification is diameter 0.1～2.0mm, length 1.0～10.0mm.
A kind of palladium-103 and iodine-125 compound seal seed source are processed the source core sealing in above-mentioned palladium-103 and iodine-125 compound seal seed source in titanium pipe or titanium alloy tube.
A kind of above-mentioned palladium-103 and iodine-125 compound seal seed method of core in a steady stream for preparing comprises the steps:
(1) inoculation of nanometer palladium crystal seed:
(a) support rod was immersed in the chloroformic solution of 0.1～5mol/L palladium 3～20 minutes, take out the back and use air blow drying, wherein palladium can be used the Palladous nitrate. or the palladium acetylacetonate replacement of same concentrations;
(b) support rod was immersed in the alkaline ammonia solution of hydrazine 3～20 minutes, the concentration of hydrazine is 0.5～10mol/L in this solution, and the concentration of ammonia is 0.1～5mol/L, and it is dry under 80～160 ℃ of temperature to take out the back;
(c) repeat (a) and (b) step 3～10 times.
This step can be replaced by following steps:
(a) carrier was immersed in the tin chloride solution of 0.01～0.1mol/L 1～10 minute;
(b) carrier was immersed in the palladium chloride solution of 1～5mmol/L 1～10 minute, wherein Palladous chloride. can be used the replacements such as Palladous nitrate., palladium, palladium acetylacetonate of same concentrations;
(c) repeat (a) and (b) step 5～10 times.
The inoculation that silver-colored rod is carried out nanometer palladium crystal seed helps initiation reaction when chemical plating, makes palladium-103 and silver be deposited on the surface of silver rod fast, uniformly.
(2) chemical plating of palladium-103 and silver: support rod is placed the mixed solution of forming by Palladous chloride., silver nitrate, disodiumedetate, ammonium hydroxide, hydrazine; Wherein contain palladium-103 in the palladium chloride solution; Regulating pH value is 6～12; Stirring reaction is 0.5～5 hour under 25～100 ℃ of condition of water bath heating, makes carrier surface evenly cover one deck palladium-103 and silver.
Palladous chloride. concentration is 1～50mmol/L in this step, and this concentration hour can not guarantee palladium-103 at the excellent surperficial uniform distribution of silver very much, influences the uniformity that single seed source dosage field distributes, and the palladium layer is blocked up when too big, the ray that too much absorption palladium-103 is emitted; Silver nitrate concentration is 0.5～25mmol/L, and the chemisorbed that this concentration hour can't provide enough silver to be used for iodine-125 very much can increase seed source itself emits ray to palladium-103 and iodine-125 self-absorption when too big; Disodiumedetate concentration is 0.1～0.5mol/L, and it act as as chelating agent and regulates silver and palladic current potential, makes silver and palladium to be deposited on simultaneously on the support rod; Ammonium hydroxide concentration is 1～10mol/L, and it act as is to regulate silver and palladic current potential as chelating agent, simultaneously also as the pH value regulator; Hydrazine concentration is 5～50mmol/L, and this concentration hour can reduce very much reaction rate and reduce the utilization rate of palladium-103, is prone to cause plating bath to decompose when too big.PH value all in 6～12 scopes, can add proper amount of sodium hydroxide as required pH value is regulated generally speaking in the solution in solution.Carrier surface area is 1～10cm with the liquor capacity ratio in this step
2/ mL.Wherein Palladous chloride. can use Palladous nitrate., palladium or the palladium acetylacetonate of same concentrations to replace, and disodiumedetate can replace with ethylenediaminetetraacetic acid.
Palladium in this step-103 can have following three kinds of modes with the chemical plating of silver:
(I) place the mixed solution of forming by the hydrazine of the ammonium hydroxide of the disodiumedetate of the silver nitrate of the Palladous chloride. of 1～50mmol/L, 0.5～25mmol/L, 0.1～0.5mol/L, 1～10mol/L, 5～50mmol/L to carry out the chemical plating of palladium and silver simultaneously support rod.Take this chemical plating mode, palladium and silver are that to be mixed into one deck equally distributed in the plated film.
(II) earlier support rod is placed the mixed solution preplating palladium of being made up of the hydrazine of the ammonium hydroxide of the disodiumedetate of the Palladous chloride. of 1～50mmol/L, 0.1～0.5mol/L, 1～10mol/L, 5～50mmol/L; And then in mixed solution, add silver nitrate; The concentration that makes silver nitrate is 0.5～25mmol/L, carries out the chemical plating of palladium and silver.Take this chemical plating mode, plated film is divided into two-layer, and internal layer is the palladium layer, and skin is the mixed layer of palladium and silver
(III) elder generation places support rod by the Palladous chloride. of 1～50mmol/L, the disodiumedetate of 0.1～0.5mol/L, the ammonium hydroxide of 1～10mol/L, the mixed solution that the hydrazine of 5～50mmol/L is formed and carries out palladic chemical plating; Take out then, place by the silver nitrate of 0.5～25mmol/L, the disodiumedetate of 0.1～0.5mol/L, the ammonium hydroxide of 1～10mol/L, the mixed solution that the hydrazine of 5～50mmol/L is formed and carry out silver-colored chemical plating.Take this chemical plating mode, plated film is divided into two-layer, and internal layer is the palladium layer, and skin is a silver layer.
This step can be replaced by following steps: support rod is placed the mixed solution of being made up of the sodium hypophosphite of the ammonium hydroxide of the ammonium chloride of the silver nitrate of the Palladous chloride. of 1～30mmol/L, 0.5～25mmol/L, 0.3～3mol/L, 0.2～2mol/L, 0.05～0.4mol/L; Wherein contain palladium-103 in the palladium chloride solution; Regulating pH value is 6～12; Stirring reaction is 0.5～5 hour under 25～90 ℃ of condition of water bath heating, and carrier surface area is 1～10cm with the liquor capacity ratio
2/ mL.Wherein Palladous chloride. can use Palladous nitrate., palladium or the palladium acetylacetonate of same concentrations to replace, and disodiumedetate can replace with ethylenediaminetetraacetic acid.
The solution pH value is general all in 6～12 scopes in this step, if the solution that disposes not in this scope, can use acetic acid or sodium hydroxide that pH value is adjusted to 6～12.
In addition, step (1) and (2) can independently be used to prepare the source core of palladium-103 sealed seed source.
(3) chemisorbed of iodine-125: support rod is put into sodium hydroxide or the potassium hydroxide of sodium iodide or potassium iodide, the 0.01～0.5mol/L of sodium bromide or potassium bromide, the 1～10mmol/L of 0.05～1mol/L, the potassium ferricyanide mixed solution of 5～50mmol/L; Wherein contain iodine-125 in sodium iodide or the liquor kalii iodide; Regulating pH value is 6～12, and stirring reaction is 5～60 minutes under 25～60 ℃ of conditions.Wherein the concentration of sodium iodide or potassium iodide hour can not guarantee iodine-125 at the excellent surperficial uniform distribution of silver very much, influences the uniformity that single seed source dosage field distributes, and can reduce the utilization rate of iodine-125 when too big.Carrier surface area is 1～10cm with the liquor capacity ratio in this step
2/ mL.The solution pH value is general all in 6～12 scopes in this step, if the solution that disposes not in this scope, can use acetic acid or sodium hydroxide that pH value is adjusted to 6～12.
Source core structure according to the prepared sealed seed source of chemical plating mode (I) in the step (2) and this step is that palladium and iodine uniform mixing are one deck; Source core structure according to the prepared sealed seed source of chemical plating mode (II) in the step (2) and this step is two-layer, and wherein internal layer is a palladium, and skin is the mixed layer of palladium and iodine; Source core structure according to the prepared sealed seed source of chemical plating mode (III) in the step (2) and this step is two-layer, and wherein internal layer is a palladium, and skin is an iodine.
In addition, this step can independently be used to prepare the source core of iodine-125 sealed seed source, is more than 15 minutes the time when the response time of chemisorbed iodine-125, and the iodine-125 conversion ratio is higher than 97%.
(3) beneficial effect
Technical scheme provided by the invention has following advantage:
(I) can successfully be fixed in palladium-103 and iodine-125 on the carrier simultaneously; And carrier surface palladium-103 is evenly distributed with iodine-125, densification, just can make both dose distribution all reach satisfied effect at whole tumor region, thereby utilize the characteristic of two kinds of nucleic more fully; Learn from other's strong points to offset one's weaknesses; Overcome and mix the shortcoming of implanting, obtain maximum lethal effect, obtain better therapeutic effect;
(II) reagent that adopts is conventional commercial reagent, and buying is convenient, and low price reduces production cost greatly;
(III) utilization rate of palladium-103 and iodine-125 is high;
(IV) in course of reaction, do not have irritative gas to produce, do not cause environmental pollution, can guarantee working environment;
(V) the response time weak point has reduced the suffered radiation dose of operator.
The specific embodiment
The embodiment that following basis is concrete further specifies the present invention.
Embodiment one
Present embodiment is most preferred technical scheme, and used reagent is analytical pure.
The source core in a kind of palladium-103 and iodine-125 compound seal seed source; With can as the metal of X ray label or nonmetal be carrier; On this carrier, cover one deck radiosiotope thin film, key is: said radiosiotope thin film is the laminated film of palladium-103 and iodine-125.Said metallic carrier is processed by wherein a kind of of silver, copper, nickel, palladium, gold or the alloy that contains this metal, and said non-metal carrier is processed by resin, plastics etc., and the carrier in the present embodiment is made from silver.Said support shapes can be bar-shaped or round shaped grain shape, and the carrier in the present embodiment is processed bar-shaped.Said support rod specification is diameter 0.1～2.0mm, length 1.0～10.0mm.Preferred diameter 0.5mm in the present embodiment, the silver rod of length 3mm is as carrier.
A kind of palladium-103 and iodine-125 compound seal seed source adopt the method for laser soldering seal that the source core sealing in above-mentioned palladium-103 and iodine-125 compound seal seed source is processed in titanium pipe or titanium alloy tube.
A kind of above-mentioned palladium-103 and iodine-125 compound seal seed method of core in a steady stream for preparing comprises the steps:
(1) inoculation of nanometer palladium crystal seed:
(a) silver rod was immersed in the chloroformic solution of 0.5mol/L palladium 15 minutes, take out the back and use air blow drying, wherein palladium can be used the Palladous nitrate. or the palladium acetylacetonate replacement of same concentrations;
(b) silver rod was immersed in the alkaline ammonia solution of hydrazine 15 minutes, the concentration of hydrazine is 2mol/L in this solution, and the concentration of ammonia is 0.2mol/L, and it is dry under 110 ℃ of temperature to take out the back;
(c) repeat (a) and (b) step 7 time, make silver-colored excellent surface coverage one deck nanometer palladium crystal seed.
(2) chemical plating of palladium-103 and silver: silver-colored rod is placed the mixed solution of forming by the hydrazine of the ammonium hydroxide of the disodiumedetate of the silver nitrate of the Palladous chloride. of 8mmol/L, 2mmol/L, 0.15mol/L, 5mol/L, 15mmol/L; Wherein contain palladium-103 in the palladium chloride solution, its radioactivity can be regulated as required.Regulating pH value is 10, puts into plating bath to the silver-colored rod of the coated with nanometre palladium crystal seed of (1) step preparation, and carrier surface area is 8cm with the liquor capacity ratio
2/ mL, stirring reaction is 2 hours under 45 ℃ of condition of water bath heating, makes the composite membrane of surface coverage one deck palladium-103 and silver.Take out the silver rod, discard surperficial clear liquid, water cleaning silver rod three times, subsequent use.Measure the radioactivity of mixed solution and supernatant respectively, calculate the adsorption efficiency of palladium-103 by following formula:
Radioactivity * 100% of the adsorption efficiency of palladium-103=(radioactivity of the radioactivity-supernatant of mixed solution)/mixed solution, the adsorption efficiency that obtains palladium-103 is 98%.
Can the mixed solution that silver-colored rod places Palladous chloride., silver nitrate, disodiumedetate, ammonium hydroxide, the hydrazine of respective concentration to form be carried out simultaneously the chemical plating of palladium and silver in this step.Also can earlier silver-colored rod be placed the mixed solution preplating palladium of being made up of Palladous chloride., disodiumedetate, ammonium hydroxide, the hydrazine of respective concentration; And then in mixed solution, add silver nitrate; The concentration that makes silver nitrate is above-mentioned respective concentration, carries out the chemical plating of palladium and silver.Can also place the mixed solution of forming by Palladous chloride., disodiumedetate, ammonium hydroxide, the hydrazine of respective concentration to carry out palladic chemical plating silver-colored rod earlier; Take out then, place the mixed solution of forming by silver nitrate, disodiumedetate, ammonium hydroxide, the hydrazine of respective concentration to carry out the chemical plating of silver.
In this step wherein Palladous chloride. can use the Palladous nitrate., palladium of same concentrations or palladium acetylacetonate to replace, disodiumedetate can replace with ethylenediaminetetraacetic acid.
(3) chemisorbed of iodine-125: silver-colored rod is put into sodium hydroxide or the potassium hydroxide of sodium iodide or potassium iodide, the 0.05mol/L of sodium bromide or potassium bromide, the 5mmol/L of 0.2mol/L, the potassium ferricyanide mixed solution of 25mmol/L; Wherein contain iodine-125 in sodium iodide or the liquor kalii iodide, its radioactivity can be regulated as required.Regulating pH value is 10, and the surface coverage palladium-103 of second step preparation and the silver-colored rod of silver composite membrane are put into solution, and carrier surface area is 8cm with the liquor capacity ratio
2/ mL, stirring reaction is 15 minutes under 25 ℃ of condition of water bath heating, takes out the silver rod, discards surperficial clear liquid, water, acetone silver rod surface three times.Measure the radioactivity of mixed solution and supernatant respectively, calculate adsorption efficiency by following formula:
Radioactivity * 100% of the adsorption efficiency of iodine-125=(radioactivity of the radioactivity-supernatant of mixed solution)/mixed solution, the adsorption efficiency that obtains iodine-125 is 99%.
Embodiment two
Other guide is constant, is with the difference part of embodiment one:
A kind of above-mentioned palladium-103 and iodine-125 compound seal seed method of core in a steady stream for preparing comprises the steps:
(1) inoculation of nanometer palladium crystal seed:
(a) silver rod was immersed in the chloroformic solution of 0.1mol/L palladium 20 minutes, take out the back and use air blow drying, wherein palladium can be used the Palladous nitrate. or the palladium acetylacetonate replacement of same concentrations;
(b) silver rod was immersed in the alkaline ammonia solution of hydrazine 20 minutes, the concentration of hydrazine is 0.5mol/L in this solution, and the concentration of ammonia is 0.1mol/L, and it is dry under 80 ℃ of temperature to take out the back;
(c) repeat (a) and (b) step 10 time, make silver-colored excellent surface coverage one deck nanometer palladium crystal seed.
(2) chemical plating of palladium-103 and silver: silver-colored rod is placed the mixed solution of forming by the hydrazine of the ammonium hydroxide of the disodiumedetate of the silver nitrate of the Palladous chloride. of 1mmol/L, 0.5mmol/L, 0.1mol/L, 1mol/L, 5mmol/L; Regulating pH value is 6; Put into plating bath to the silver-colored rod of the coated with nanometre palladium crystal seed of (1) step preparation, carrier surface area is 1cm with the liquor capacity ratio
2/ mL, stirring reaction is 0.5 hour under 100 ℃ of condition of water bath heating, makes the composite membrane of surface coverage one deck palladium-103 and silver.Take out the silver rod, discard surperficial clear liquid, water cleaning silver rod three times, subsequent use.Calculating palladium-103 adsorption efficiency by embodiment 1 method is 96%.
(3) chemisorbed of iodine-125: silver-colored rod is put into sodium hydroxide or the potassium hydroxide of sodium iodide or potassium iodide, the 0.01mol/L of sodium bromide or potassium bromide, the 1mmol/L of 0.05mol/L, the potassium ferricyanide mixed solution of 5mmol/L; PH value is 6; The surface coverage palladium-103 of second step preparation and the silver-colored rod of silver composite membrane are put into solution, and carrier surface area is 1cm with the liquor capacity ratio
2/ mL, stirring reaction is 60 minutes under 45 ℃ of conditions, takes out the silver rod, discards surperficial clear liquid, water, acetone silver rod surface each three times.Calculating the iodine-125 adsorption efficiency by embodiment 1 method is 97%.
Embodiment three
Other guide is constant, is with the difference part of embodiment one:
A kind of above-mentioned palladium-103 and iodine-125 compound seal seed method of core in a steady stream for preparing comprises the steps:
(1) inoculation of nanometer palladium crystal seed:
(a) silver rod was immersed in the chloroformic solution of 5mol/L palladium 3 minutes, take out the back and use air blow drying, wherein palladium can be used the Palladous nitrate. or the palladium acetylacetonate replacement of same concentrations;
(b) silver rod was immersed in the alkaline ammonia solution of hydrazine 3 minutes, the concentration of hydrazine is 10mol/L in this solution, and the concentration of ammonia is 5mol/L, and it is dry under 160 ℃ of temperature to take out the back;
(c) repeat (a) and (b) step 3 time, make silver-colored excellent surface coverage one deck nanometer palladium crystal seed.
(2) chemical plating of palladium-103 and silver: silver-colored rod is placed the mixed solution of forming by the hydrazine of the ammonium hydroxide of the disodiumedetate of the silver nitrate of the Palladous chloride. of 50mmol/L, 25mmol/L, 0.5mol/L, 10mol/L, 50mmol/L; Regulating pH value is 12; Put into plating bath to the silver-colored rod of the coated with nanometre palladium crystal seed of (1) step preparation, carrier surface area is 1cm with the liquor capacity ratio
2/ mL, stirring reaction is 5 hours under 25 ℃ of condition of water bath heating, makes the composite membrane of surface coverage one deck palladium-103 and silver.Take out the silver rod, discard surperficial clear liquid, water cleaning silver rod three times, subsequent use.Calculating palladium-103 adsorption efficiency by embodiment 1 method is 95%.
(3) chemisorbed of iodine-125: silver-colored rod is put into sodium hydroxide or the potassium hydroxide of sodium iodide or potassium iodide, the 0.5mol/L of sodium bromide or potassium bromide, the 10mmol/L of 1mol/L, the potassium ferricyanide mixed solution of 50mmol/L; PH value is 12; The surface coverage palladium-103 of second step preparation and the silver-colored rod of silver composite membrane are put into solution, and carrier surface area is 10cm with the liquor capacity ratio
2/ mL, stirring reaction is 5 minutes under 60 ℃ of conditions, takes out the silver rod, discards surperficial clear liquid, water, acetone silver rod surface each three times.Calculating the iodine-125 adsorption efficiency by embodiment 1 method is 98%.
Embodiment four
Other guide is constant, is with the difference of embodiment one, and the inoculation of nanometer palladium crystal seed is in the step (1):
(a) silver rod was immersed in the tin chloride solution of 0.1mol/L 1 minute;
(b) silver rod was immersed in the palladium chloride solution of 5mmol/L 1 minute, wherein Palladous chloride. can be used the replacements such as Palladous nitrate., palladium, palladium acetylacetonate of same concentrations;
(c) repeat (a) and (b) step 5 time, make silver-colored excellent surface coverage one deck nanometer palladium crystal seed.
Embodiment five
Other guide is constant, is with the difference of embodiment one, and the inoculation of nanometer palladium crystal seed is in the step (1):
(a) silver rod was immersed in the tin chloride solution of 0.05mol/L 5 minutes;
(b) silver rod was immersed in the palladium chloride solution of 3mmol/L 5 minutes, wherein Palladous chloride. can be used the replacements such as Palladous nitrate., palladium, palladium acetylacetonate of same concentrations;
(c) repeat (a) and (b) step 8 time, make silver-colored excellent surface coverage one deck nanometer palladium crystal seed.
Embodiment six
Other guide is constant, is with the difference of embodiment one, and the inoculation of nanometer palladium crystal seed is in the step (1):
(a) silver rod was immersed in the tin chloride solution of 0.01mol/L 10 minutes;
(b) silver rod was immersed in the palladium chloride solution of 1mmol/L 10 minutes, wherein Palladous chloride. can be used the replacements such as Palladous nitrate., palladium, palladium acetylacetonate of same concentrations;
(c) repeat (a) and (b) step 10 time, make silver-colored excellent surface coverage one deck nanometer palladium crystal seed.
Embodiment seven
Other guide is constant; Be with the difference of embodiment one; Palladium-103 with the chemical plating of silver is in the step (2): silver-colored rod is placed the mixed solution of being made up of the sodium hypophosphite of the ammonium hydroxide of the ammonium chloride of the silver nitrate of the Palladous chloride. of 10mmol/L, 5mmol/L, 0.5mol/L, 2.5mol/L, 0.1mol/L; Regulating pH value is 10, and stirring reaction is 2 hours under 60 ℃ of condition of water bath heating, and wherein carrier surface area is 6cm with the liquor capacity ratio
2/ mL.Wherein Palladous chloride. can use Palladous nitrate., palladium or the palladium acetylacetonate of same concentrations to replace, and disodiumedetate can replace with ethylenediaminetetraacetic acid.
Embodiment eight
Other guide is constant; Be with the difference of embodiment one; Palladium-103 with the chemical plating of silver is in the step (2): silver-colored rod is placed the mixed solution of being made up of the sodium hypophosphite of the ammonium hydroxide of the ammonium chloride of the silver nitrate of the Palladous chloride. of 1mmol/L, 0.5mmol/L, 0.2mol/L, 0.3mol/L, 0.05mol/L; Regulating pH value is 6, and stirring reaction is 5 hours under 25 ℃ of condition of water bath heating, and carrier surface area is 1cm with the liquor capacity ratio
2/ mL.Wherein Palladous chloride. can use Palladous nitrate., palladium or the palladium acetylacetonate of same concentrations to replace, and disodiumedetate can replace with ethylenediaminetetraacetic acid.
Embodiment nine
Other guide is constant; Be with the difference of embodiment one; Palladium-103 with the chemical plating of silver is in the step (2): silver-colored rod is placed the mixed solution of being made up of the sodium hypophosphite of the ammonium hydroxide of the ammonium chloride of the silver nitrate of the Palladous chloride. of 30mmol/L, 20mmol/L, 2mol/L, 3mol/L, 0.4mol/L; Regulating pH value is 12, and stirring reaction is 0.5 hour under 100 ℃ of condition of water bath heating, and carrier surface area is 1～10cm with the liquor capacity ratio
2/ mL.Wherein Palladous chloride. can use Palladous nitrate., palladium or the palladium acetylacetonate of same concentrations to replace, and disodiumedetate can replace with ethylenediaminetetraacetic acid.
Embodiment ten
The used reagent of present embodiment is analytical pure.
The source core in a kind of palladium-103 and iodine-125 compound seal seed source; With can as the metal of X ray label or nonmetal be carrier; On this carrier, cover one deck radiosiotope thin film, key is: said radiosiotope thin film is the laminated film of palladium-103 and iodine-125.Said metallic carrier is processed by wherein a kind of of silver, copper, nickel, palladium, gold or the alloy that contains this metal, and said non-metal carrier is by resin, plastics etc.
SystemBecome, the carrier in the present embodiment is made from silver.Said support shapes can be bar-shaped or round shaped grain shape, and the carrier in the present embodiment is processed bar-shaped.Said support rod specification is diameter 0.1～2.0mm, length 1.0～10.0mm.Preferred diameter 0.5mm in the present embodiment, the silver rod of length 3mm is as carrier.
A kind of palladium-103 and iodine-125 compound seal seed source adopt the method for laser soldering seal that the source core sealing in above-mentioned palladium-103 and iodine-125 compound seal seed source is processed in titanium pipe or titanium alloy tube.
A kind of above-mentioned palladium-103 and iodine-125 compound seal seed method of core in a steady stream for preparing comprises the steps:
(1) chemical plating of palladium-103 and silver: silver-colored rod is placed the mixed solution of forming by the hydrazine of the ammonium hydroxide of the disodiumedetate of the silver nitrate of the Palladous chloride. of 8mmol/L, 2mmol/L, 0.15mol/L, 5mol/L, 15mmol/L; Regulating pH value is 10; Silver-colored rod is put into plating bath, and carrier surface area is 8cm with the liquor capacity ratio
2/ mL, stirring reaction is 5 hours under 45 ℃ of condition of water bath heating, makes the composite membrane of surface coverage one deck palladium-103 and silver.Take out the silver rod, discard surperficial clear liquid, water cleaning silver rod three times, subsequent use.
Can the mixed solution that silver-colored rod places Palladous chloride., silver nitrate, disodiumedetate, ammonium hydroxide, the hydrazine of respective concentration to form be carried out simultaneously the chemical plating of palladium and silver in this step.Also can earlier silver-colored rod be placed the mixed solution preplating palladium of being made up of Palladous chloride., disodiumedetate, ammonium hydroxide, the hydrazine of respective concentration; And then in mixed solution, add silver nitrate; The concentration that makes silver nitrate is above-mentioned respective concentration, carries out the chemical plating of palladium and silver.Can also place the mixed solution of forming by Palladous chloride., disodiumedetate, ammonium hydroxide, the hydrazine of respective concentration to carry out palladic chemical plating silver-colored rod earlier; Take out then, place the mixed solution of forming by silver nitrate, disodiumedetate, ammonium hydroxide, the hydrazine of respective concentration to carry out the chemical plating of silver.
In this step wherein Palladous chloride. can use the Palladous nitrate., palladium of same concentrations or palladium acetylacetonate to replace, disodiumedetate can replace with ethylenediaminetetraacetic acid.
(2) chemisorbed of iodine-125: the silver-colored rod of preparation in the step (1) is put into sodium hydroxide or the potassium hydroxide of sodium iodide or potassium iodide, the 0.05mol/L of sodium bromide or potassium bromide, the 5mmol/L of 0.2mol/L, the potassium ferricyanide mixed solution of 25mmol/L; PH value is 10; The surface coverage palladium-103 of second step preparation and the silver-colored rod of silver composite membrane are put into solution, and carrier surface area is 8cm with the liquor capacity ratio
2/ mL, stirring reaction is 15 minutes under 25 ℃ of condition of water bath heating, takes out the silver rod, discards surperficial clear liquid, water, acetone silver rod surface three times.
Above content is to combine preferred embodiment to specify what the present invention did, can not assert that the specific embodiment of the present invention only limits to these explanations.Under the present invention, the those of ordinary skill of technical field, under the prerequisite that does not break away from the present invention's design, can also make some simple deductions and conversion, all should be regarded as belonging to protection scope of the present invention.
Claims (10)
1. a palladium-103 and the iodine-125 compound seal seed method for preparing of core in a steady stream comprises the steps:
(1) chemical plating of palladium-103 and silver: support rod is placed the mixed solution of forming by the hydrazine of the ammonium hydroxide of the disodiumedetate of the silver nitrate of the Palladous chloride. of 1～50mmol/L, 0.5～25mmol/L, 0.1～0.5mol/L, 1～10mol/L, 5～50mmol/L; Wherein contain palladium-103 in the palladium chloride solution; Regulating pH value is 6～12, and stirring reaction is 0.5～5 hour under 25～100 ℃ of condition of water bath heating;
(2) chemisorbed of iodine-125: support rod is put into sodium hydroxide or the potassium hydroxide of sodium iodide or potassium iodide, the 0.01～0.5mol/L of sodium bromide or potassium bromide, the 1～10mmol/L of 0.05～1mol/L, the potassium ferricyanide mixed solution of 5～50mmol/L; Wherein contain iodine-125 in sodium iodide or the liquor kalii iodide; Regulating pH value is 6～12, and stirring reaction is 5～60 minutes under 25～60 ℃ of conditions.
2. method for preparing according to claim 1 is characterized in that: place the mixed solution of being made up of the hydrazine of the ammonium hydroxide of the disodiumedetate of the silver nitrate of the Palladous chloride. of 1～50mmol/L, 0.5～25mmol/L, 0.1～0.5mol/L, 1～10mol/L, 5～50mmol/L to carry out the chemical plating of palladium and silver simultaneously support rod in the step (1); Perhaps earlier support rod is placed the mixed solution preplating palladium of being made up of the hydrazine of the ammonium hydroxide of the disodiumedetate of the Palladous chloride. of 1～50mmol/L, 0.1～0.5mol/L, 1～10mol/L, 5～50mmol/L; And then in mixed solution, add silver nitrate; The concentration that makes silver nitrate is 0.5～25mmol/L, carries out the chemical plating of palladium and silver; Perhaps earlier support rod is placed by the Palladous chloride. of 1～50mmol/L, the disodiumedetate of 0.1～0.5mol/L, the ammonium hydroxide of 1～10mol/L, the mixed solution that the hydrazine of 5～50mmol/L is formed and carry out palladic chemical plating; Take out then, place by the silver nitrate of 0.5～25mmol/L, the disodiumedetate of 0.1～0.5mol/L, the ammonium hydroxide of 1～10mol/L, the mixed solution that the hydrazine of 5～50mmol/L is formed and carry out silver-colored chemical plating.
3. method for preparing according to claim 1 is characterized in that: in step (1) and (2), the support rod surface area is 1～10cm with the liquor capacity ratio
2/ mL.
4. according to each described method for preparing of claim 1 to 3, it is characterized in that, also comprise the step of the inoculation of nanometer palladium crystal seed in step (1) before:
(a) support rod was immersed in the chloroformic solution of 0.1～5mol/L palladium 3～20 minutes, take out the back and use air blow drying;
(b) support rod was immersed in the alkaline ammonia solution of hydrazine 3～20 minutes, the concentration of hydrazine is 0.5～10mol/L in this solution, and the concentration of ammonia is 0.1～5mol/L, and it is dry under 80～160 ℃ of temperature to take out the back;
(c) repeat (a) and (b) step 3～10 times.
5. according to each described method for preparing of claim 1 to 3, it is characterized in that, also comprise the step of the inoculation of nanometer palladium crystal seed in step (1) before:
(a) support rod was immersed in the tin chloride solution of 0.01～0.1mol/L 1～10 minute;
(b) support rod was immersed in the palladium chloride solution of 1～5mmol/L 1～10 minute;
(c) repeat (a) and (b) step 5～10 times.
6. a palladium-103 and the iodine-125 compound seal seed method for preparing of core in a steady stream comprises the steps:
(1) chemical plating of palladium-103 and silver: support rod is placed the mixed solution of forming by the sodium hypophosphite of the ammonium hydroxide of the ammonium chloride of the silver nitrate of the Palladous chloride. of 1～30mmol/L, 0.5～25mmol/L, 0.3～3mol/L, 0.2～2mol/L, 0.05～0.4mol/L; Wherein contain palladium-103 in the palladium chloride solution; Regulating pH value is 6～12, and stirring reaction is 0.5～5 hour under 25～90 ℃ of condition of water bath heating;
(2) chemisorbed of iodine-125: support rod is put into sodium hydroxide or the potassium hydroxide of sodium iodide or potassium iodide, the 0.01～0.5mol/L of sodium bromide or potassium bromide, the 1～10mmol/L of 0.05～1mol/L, the potassium ferricyanide mixed solution of 5～50mmol/L; Wherein contain iodine-125 in sodium iodide or the liquor kalii iodide; Regulating pH value is 6～12, and stirring reaction is 5～60 minutes under 25～60 ℃ of conditions.
7. method for preparing according to claim 6 is characterized in that, also comprises the step of the inoculation of nanometer palladium crystal seed before in step (1):
(a) support rod was immersed in the chloroformic solution of 0.1～5mol/L palladium 3～20 minutes, take out the back and use air blow drying;
(b) support rod was immersed in the alkaline ammonia solution of hydrazine 3～20 minutes, the concentration of hydrazine is 0.5～10mol/L in this solution, and the concentration of ammonia is 0.1～5mol/L, and it is dry under 80～160 ℃ of temperature to take out the back;
(c) repeat (a) and (b) step 3～10 times.
8. one kind is adopted the palladium-103 that claim 1 or 6 described methods make and the source core in iodine-125 compound seal seed source; On support rod, cover one deck radiosiotope thin film, it is characterized in that: said radiosiotope thin film is the laminated film that contains palladium-103 and iodine-125.
9. the source core in compound seal seed according to claim 9 source is characterized in that: said support rod is processed by wherein a kind of of silver, copper, nickel, palladium, gold or the alloy that contains this metal.
10. palladium-103 and iodine-125 compound seal seed source, sealing has the radioactivity source core in titanium pipe or titanium alloy tube, it is characterized in that: said radioactivity source core is the source core in palladium described in the claim 8-103 and iodine-125 compound seal seed source.
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| WO2012000134A1 (en) * | 2010-07-01 | 2012-01-05 | Zhang Jianguo | Composite type radioactive isotope sealed seed source |
| CN103301560A (en) * | 2012-03-16 | 2013-09-18 | 吴沛宏 | Radioactive particles for treating tumor and implantation method |
| CN103705948B (en) * | 2013-12-10 | 2015-09-23 | 原子高科股份有限公司 | A kind of source core carrier of radioactive particle and preparation technology thereof |
| CN104127917B (en) * | 2014-07-08 | 2016-06-08 | 原子高科股份有限公司 | A kind of radiant stand and preparation method thereof |
| CN104127915B (en) * | 2014-07-08 | 2016-08-17 | 原子高科股份有限公司 | A kind of compound nucleic radiant stand and preparation method thereof |
| CN105031676B (en) * | 2015-07-07 | 2018-06-29 | 原子高科股份有限公司 | It is a kind of131Cs particles and its preparation process |
| CN108498939B (en) * | 2017-02-28 | 2020-08-25 | 武汉大学 | Radioactive particles capable of self-fixing position |
| CN109754890B (en) * | 2018-12-26 | 2020-11-03 | 北京工业大学 | Method for manufacturing radioactive seed source core by utilizing electrohydrodynamic micro-droplet injection |
| CN112972708A (en) * | 2021-02-22 | 2021-06-18 | 姜伟 | Palladium-103 and iodine-125 composite sealed seed source, source core and source core preparation method |
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