CN106540282A - A kind of preparation method of -103 sealed seed source source core of palladium - Google Patents

A kind of preparation method of -103 sealed seed source source core of palladium Download PDF

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CN106540282A
CN106540282A CN201510591213.0A CN201510591213A CN106540282A CN 106540282 A CN106540282 A CN 106540282A CN 201510591213 A CN201510591213 A CN 201510591213A CN 106540282 A CN106540282 A CN 106540282A
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palladium
source
sealed seed
preparation
seed source
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CN106540282B (en
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阎尔坤
白红升
张兴福
朱辉
李佳
崔贝
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TIANJIN SAIDE BIOLOGICAL PHARMACEUTICAL CO Ltd
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TIANJIN SAIDE BIOLOGICAL PHARMACEUTICAL CO Ltd
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Abstract

The invention discloses a kind of preparation method of -103 sealed seed source source core of palladium, is made up of following steps:In reaction vessel, 100 silver-colored rods are put in proportion, add saline citrate, soluble palladium saline solution and sodium hydrate aqueous solution, mixing, reaction, is subsequently adding -103 aqueous solution of radioactivity palladium bichloride and aqueous thiosulfate, in the lower oscillating reactions in pH=6~11, supernatant is abandoned, with acetone, deionized water or ethanol purge, that is, -103 sealed seed source source core of palladium is obtained.Method of the present invention reaction system is stable, -103 sealed seed source source core dose uniformity of palladium of preparation, firmly and fine and close, -103 utilization rate of palladium height.Reaction time is short, and whole preparation process at most needs 60min, and one-step method is completed at ambient temperature, and operational sequence is simple and easy to control, improves production efficiency, reduces labour intensity and dose of radiation.The chemical reagent for being used is conventional commercial, nontoxic, low price, low production cost.

Description

A kind of preparation method of -103 sealed seed source source core of palladium
Technical field
The invention belongs to contain the medicinal preparation technical field of radioactive substance, specifically being related to a kind of -103 sealed seed source of palladium The preparation method of source core.
Background technology
Radioactive particle Implantation in Treating tumour be by art or using implanting device percutaneous puncture by radioactive particle (radiation Property sealed seed source) around implantation tumour or tumour, it is thin that the low-energyγ-ray released using radionuclide or X-ray kill tumour Born of the same parents, reach treatment and alleviate the purpose of disease.The technology is adapted to the implanted treatment of various entity tumors, such as prostate cancer, breast Gland cancer, liver cancer, incidence knurl, cancer of pancreas and oophoroma etc., achieve and control curative effect with surgical operation, fluconazole ear drops identical Really, with Small side effects, recurrence rate be low and wound is little etc..The most frequently used radioactive particle of the technology is that iodine-125 seals seed at present - 103 sealed seed source of source and palladium, wherein iodine-125 sealed seed source are applied to the tumor implantation therapy of growth is slow;Palladium -103 seals seed Source is applied to the fast tumor implantation therapy of growth.
Compared with other radionuclides, radionuclide palladium -103 have good nulcear properties, palladium [103Pd] do not have volatility, Therefore the pollution to operating environment around and personnel can effectively be avoided;Next, palladium [103Pd] energy is low, only 21~23KeV Characteristic X-ray, easily shield, the lead of 0.06 millimeters thick it is prevented that more than 97% ray is passed through, half in tissue Subtract layer for 1 centimetre, therefore protection is more convenient, exposure dose suffered by normal structure and surrounding population is little;3rd, palladium [103Pd] Half-life short, the half-life of 16.96 days can make the predose height of implantation, and doses remaining is little, swollen for suppression fast-growth Knurl has good therapeutic effect.
- 103 sealed seed source of palladium is that the support rod (also referred to as -103 source core of radioactivity palladium) for being adsorbed with palladium -103 is loaded titanium tube or not Rust steel pipe in, sealing two ends and made by.
Support rod for preparing -103 sealed seed source of palladium is resin microsphere, ceramic rod or microballoon, inorganic adsorbent microballoon and metal bar (gold, silver, copper etc.), generally selects silver as the support rod of fixed palladium -103, as the ductility of argent is easily worked, Price is low, and is the mark of x-ray, -103 sealed seed source of palladium is accurately positioned and therapeutic agent when being easy to implanted treatment The estimation of amount.Different tumor implantation therapies are used for according to -103 sealed seed source of palladium, the length of silver-colored rod is 3.0mm, a diameter of Φ 0.1~0.7mm, it is that palladium -103 is close that radionuclide palladium -103 is fixed on the technology (also referred to as -103 source core technology of preparing of palladium) of silver-colored rod The key technology of envelope seed source manufacture, generally has absorption method, galvanoplastic and electroless plating method.Compared with other two kinds, chemical plating has Technological process is simple, the utilization rate of palladium -103 is high, equipment is easily obtained, preparation process has been controlled and easily large-scale production.For example it is beautiful State's patent US4702228 discloses a kind of absorption method, for the Adsorption of Radioactive such as aluminum oxide micro-sphere palladium -103, by absorption after two Individual microballoon loads titanium tube, and -103 sealed seed source of palladium that silver-colored rod is prepared as x-ray mark, the method is inserted between two microballoons Active region at the two ends of sealed seed source, it is difficult to ensure that dosage distributing homogeneity, process is wayward, while it is close to increase palladium -103 The difficulty of envelope seed source assembling, is difficult large-scale production, while dosage distribution changes because of the movement of two microballoons, to clinic Therapeutic effect is produced and does not utilize impact, is difficult to realize the accurate treatment of tumour.Chinese patent Zl01105243.0 discloses a kind ofization Plating method is learned, with palladium bichloride, ammonium chloride, ammoniacal liquor and sodium hypophosphite as main solution composition, is reacted 1 hour at pH=10 and 35 DEG C, Make silver-colored rod surface cover last layer palladium -103, that is, -103 source core of palladium is obtained.The method is using ammonium chloride as stabilizer, but ammonium chloride Reaction rate can be reduced while plating solution is stablized, the concentration of required reducing agent sodium hypophosphite is higher in addition, is unfavorable for plating solution Stability.Such as Chinese patent ZL101880873A discloses a kind of two-step method electroless plating method, the rod activation of (1) silver again:First will Silver-colored rod is soaked in palladium chloride aqueous solution, and taking-up is cleaned with water, is then soaked in the alkaline ammoniacal liquor of hydrazine, is cleaned with water;(2) - 103 chemical plating of palladium:The mixing that silver-colored rod after by activation is placed in palladium bichloride, sodium ethylene diamine tetracetate, ammonium hydroxide and hydrazine composition is molten In liquid, 30~90min of stirring reaction under condition of water bath heating is prepared into -103 source core of palladium.The method reaction system is relatively stable, Complex operation, needs heating, has ammonia to discharge in course of reaction.
The content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art, there is provided a kind of low cost, easily-controllable, quick, easy palladium -103 are close The preparation method of envelope seed core in a steady stream.
Technical scheme is summarized as follows:
A kind of preparation method of -103 sealed seed source source core of palladium, is made up of following steps:
In reaction vessel, the silver-colored rod that 100 a diameter of 0.1~0.7mm, length are 2.0~3.5mm is put in proportion, plus Enter 0.01~2mL concentration be the saline citrate of 0.01~2mol/L, 0.1~2mL concentration be 0.003~0.06mol/L Soluble palladium saline solution and 0.01~1mL concentration are 0.02~2mol/L sodium hydrate aqueous solutions, are mixed, and are reacted 1~5 minute, Being subsequently adding 0.1~1mL concentration for -103 aqueous solution of 100-1000mCi/mL radioactivity palladium bichloride and 0.1~2mL concentration is 0.05mol/L~1.0mol/L aqueous thiosulfates, in 20~60min of the lower oscillating reactions in pH=6~11, abandon supernatant, use Acetone, deionized water or ethanol purge 2~4 times, that is, obtain -103 sealed seed source source core of palladium.
Citrate optimization citric acid sodium or potassium citrate.
The preferred palladium bromide of soluble palladium salt, fluorination palladium or palladium bichloride.
The preferred sodium thiosulfate of thiosulfate or potassium thiosulfate.
Advantages of the present invention:
1. the method for the present invention is adopted soluble palladium saline solution, saline citrate, sodium hydrate aqueous solution and thio sulphur The reaction system of acid salt aqueous solution composition, reaction system is stable, -103 sealed seed source source core dose uniformity of palladium of preparation, firmly and Densification, -103 utilization rate of palladium are high.
2. the method for the present invention reaction time is short, and whole preparation process at most needs 60min, and one-step method is completed at ambient temperature, Operational sequence is simple and easy to control, substantially increases production efficiency, reduces the labour intensity and dose of radiation of staff.
3. the chemical reagent used by the method for the present invention is conventional commercial reagent, and nontoxic, buying is convenient, and low price is raw Produce low cost.
Description of the drawings
Fig. 1 is -103 sealed seed source structural representation of palladium.
In figure, 1 is titanium tube, and 2 is -103 sealed seed source source core of palladium.
Specific embodiment
With reference to specific enforcement, the present invention is further illustrated.
It is pure that chemical reagent used in all embodiments is analysis.
Embodiment 1
A kind of preparation method of -103 sealed seed source source core of palladium, is made up of following steps:
100 silver-colored rods (0.3 × 3mm of Φ) are loaded into the reaction bulb of 15mL, adds 0.2mL 0.1mol/L sodium citrates water-soluble Liquid, 0.3mL0.02mol/L palladium chloride aqueous solutions and 0.5mL0.04mol/L sodium hydrate aqueous solutions, mixing react 2min, - 103 aqueous solution of 1mL 100mCi/mL radioactivity palladium bichloride and 0.1mL 1.0mol/L sodium thiosulfate solutions are added, is adjusted PH=10, oscillating reactions 30 minutes abandon supernatant, and deionized water is cleaned 3 times, dries, that is, obtain -103 sealed seed source source of palladium Core.Then the source core made is loaded in the titanium tube of Φ 0.5mm, uses laser welder sealing, see Fig. 1.
After reaction, in solution, the activity of palladium -103 is 0.4mCi, and the utilization rate of palladium -103 is 99.6%, -103 source core of palladium it is average Radioactive activity is 0.730mCi.
The utilization rate of palladium -103=[activity of palladium -103 (after the activity-reaction of input palladium -103 in solution) ÷ input palladiums -103 Activity] × 100%.
Embodiment 2
A kind of preparation method of -103 sealed seed source source core of palladium, is made up of following steps:
100 silver-colored rods (0.5 × 3mm of Φ) are loaded into the reaction bulb of 15mL, add 0.01mL 2mol/L sodium citrate aqueous solutions, 0.1mL 0.06mol/L palladium chloride aqueous solutions and 0.01mL 2mol/L sodium hydrate aqueous solutions, mixing, reaction 1min, then plus Enter -103 aqueous solution of 0.1mL 1000mCi/mL radioactivity palladium bichloride and 0.1mL 1.0mol/L sodium thiosulfate solutions, adjust PH=6, oscillating reactions 60 minutes, abandons supernatant, is cleaned with acetone 2 times, is dried, that is, obtain -103 sealed seed source source core of palladium. Then the source core made is loaded in the titanium tube of Φ 0.8mm, uses laser welder sealing.
After reaction, in solution, the activity of palladium -103 is 0.75mCi, and the utilization rate of palladium -103 is 99.25%, -103 source core of palladium it is flat Radioactive activity is 0.65mCi.
Embodiment 3
A kind of preparation method of -103 sealed seed source source core of palladium, is made up of following steps:
100 silver-colored rods (0.7 × 2mm of Φ) are loaded into the square quartzy bottle of 15mL, 2mL 0.01mol/L potassium citrate water is added Solution, 2mL0.003mol/L palladium chloride aqueous solutions and 1mL 0.02mol/L sodium hydrate aqueous solutions, mixing react 5min, - 103 aqueous solution of 1mL 180mCi/mL radioactivity palladium bichloride and 2mL 0.05mol/L thiosulfuric acid aqueous solutions of potassium are added, is adjusted PH=11, oscillating reactions 40 minutes, abandons supernatant, with ethanol purge 2 times, dries, that is, obtains -103 sealed seed source source core of palladium. Then the source core made is loaded in the titanium tube of Φ 1.0mm, uses laser welder sealing.
After reaction, in solution, the activity of palladium -103 is 0.70mCi, and the utilization rate of palladium -103 is 99.61%, -103 source core of palladium Mean radio activity is 1.05mCi.
Embodiment 4
A kind of preparation method of -103 sealed seed source source core of palladium, is made up of following steps:
100 silver-colored rods (0.1 × 3.5mm of Φ) are loaded into the square quartzy bottle of 15mL, 0.4mL 0.05mol/L citric acids are added Aqueous solutions of potassium, 0.4mL0.015mol/L fluorination aqueous palladiums and 0.4mL 0.05mol/L sodium hydrate aqueous solutions, mixing, instead 4min is answered, -103 aqueous solution of 0.5mL 200mCi/mL radioactivity palladium bichloride and 0.4mL 0.25mol/L potassium thiosulfates is added The aqueous solution, adjusts pH=11, and supernatant is abandoned in oscillating reactions 20 minutes, and deionized water is cleaned 4 times, dries, that is, obtain palladium -103 Sealed seed source source core.Then the source core made is loaded in the titanium tube of 0.3mm (Φ 0.3mm), uses laser welder sealing.
After reaction, in solution, the activity of palladium -103 is 0.8mCi, and the utilization rate of palladium -103 is 99.2%, -103 source core of palladium it is average Radioactive activity is 0.625mCi.
Embodiment 5
A kind of preparation method of -103 sealed seed source source core of palladium, is made up of following steps:
100 silver-colored rods (0.7 × 3.5mm of Φ) are loaded into the square quartzy bottle of 15mL, 0.4mL 0.05mol/L citric acids are added Aqueous solutions of potassium, 0.4mL0.015mol/L brominations aqueous palladium and 0.4mL 0.05mol/L sodium hydrate aqueous solutions, mixing, instead 4min is answered, -103 aqueous solution of 0.5mL 100mCi/mL radioactivity palladium bichloride and 0.4mL 0.25mol/L sodium thiosulfate is added The aqueous solution, adjusts pH=10, and supernatant is abandoned in oscillating reactions 35 minutes, and deionized water is cleaned 3 times, dries, that is, obtain palladium -103 Sealed seed source source core.Then the source core made is loaded in the titanium tube of 1.0mm (Φ 1.0mm), uses laser welder sealing.
After reaction, in solution, the activity of palladium -103 is 0.25mCi, and the utilization rate of palladium -103 is 99.5%, -103 source core of palladium it is average Radioactive activity is 0.41mCi.
Above content is to illustrating that the present invention is done with reference to the embodiment for optimizing, it is impossible to assert embodiments of the present invention only Existing these explanations.For the different technologies personnel of the technical field of the invention, without departing from the inventive concept of the premise, Some simple deductions and conversion can also be made, should be all considered as belonging in protection scope of the present invention.

Claims (4)

1. a kind of preparation method of -103 sealed seed source source core of palladium, is characterized in that being made up of following steps:
In reaction vessel, the silver-colored rod that 100 a diameter of 0.1~0.7mm, length are 2.0~3.5mm is put in proportion, plus Enter 0.01~2mL concentration be the saline citrate of 0.01~2mol/L, 0.1~2mL concentration be 0.003~0.06mol/L Soluble palladium saline solution and 0.01~1mL concentration are 0.02~2mol/L sodium hydrate aqueous solutions, are mixed, and are reacted 1~5 minute, Being subsequently adding 0.1~1mL concentration for -103 aqueous solution of 100-1000mCi/mL radioactivity palladium bichloride and 0.1~2mL concentration is 0.05mol/L~1.0mol/L aqueous thiosulfates, in 20~60min of the lower oscillating reactions in pH=6~11, abandon supernatant, use Acetone, deionized water or ethanol purge 2~4 times, that is, obtain -103 sealed seed source source core of palladium.
2. a kind of preparation method of -103 sealed seed source source core of palladium according to claim 1, is characterized in that the citrate is lemon Lemon acid sodium or potassium citrate.
3. a kind of preparation method of -103 sealed seed source source core of palladium according to claim 1, is characterized in that the soluble palladium salt is Palladium bromide, fluorination palladium or palladium bichloride.
4. a kind of preparation method of -103 sealed seed source source core of palladium according to claim 1, is characterized in that the thiosulfate is Sodium thiosulfate or potassium thiosulfate.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101469420A (en) * 2007-04-16 2009-07-01 上村工业株式会社 Electroless gold-plating method and electronic component
CN101709462A (en) * 2009-12-23 2010-05-19 长沙理工大学 Chemical palladium plating solution
CN101880873A (en) * 2010-06-30 2010-11-10 中国原子能科学研究院 103Preparation process of Pd sealed seed source core
CN104561943A (en) * 2014-12-27 2015-04-29 广东致卓精密金属科技有限公司 Chemical nickel-palladium alloy plating process for circuit boards

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101469420A (en) * 2007-04-16 2009-07-01 上村工业株式会社 Electroless gold-plating method and electronic component
CN101709462A (en) * 2009-12-23 2010-05-19 长沙理工大学 Chemical palladium plating solution
CN101880873A (en) * 2010-06-30 2010-11-10 中国原子能科学研究院 103Preparation process of Pd sealed seed source core
CN104561943A (en) * 2014-12-27 2015-04-29 广东致卓精密金属科技有限公司 Chemical nickel-palladium alloy plating process for circuit boards

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