A method for separation and purification using a combination of gel resin and cationic resin 68 Ge's method

Abstract

This invention relates to a method for separation and purification using a combination of gel resin and cationic resin. 68 The method described in this invention, belonging to the field of nuclear technology applications, solves the problem that existing separation and purification methods cannot achieve one-step separation and purification, resulting in low separation and purification efficiency. The separation and purification method of this invention is as follows: Step (a): Dissolve and leach the gallium target after accelerator irradiation to obtain a feed solution; Step (b): Adjust the pH of the feed solution to alkaline; Step (c): Pass the alkaline feed solution through a gel resin column; Step (d): Elute the gel resin column; Step (e): Remove the contents containing... 68 The eluent of Ge was passed through a cation exchange resin column and washed to obtain... 68 Ge eluent. This invention achieves the [missing information - likely related to elution]. 68 One-step separation and purification of Ge.

Description

Technical Field

[0001] This invention relates to the field of nuclear technology applications, and more particularly to a method for separation and purification using a combination of gel resin and cation exchange resin. 68 Ge's method. Background Technology

[0002] 68 Ge nuclides can be used to prepare radiopharmaceuticals. Current techniques typically employ... nat Ga(p, xn) 68 Ge nuclear reaction proceeds 68 The production of Ge nuclides. Specifically, the above-mentioned production method involves irradiating natural Ga with high-energy protons, and the reaction takes place in a cyclotron.

[0003] Separation from the irradiated target 68 Germanium tetrachloride is mainly separated from other metallic impurities through solvent extraction and selective evaporation. Germanium tetrachloride is highly volatile, and this volatility has been utilized in distillation methods to separate it from other metallic impurities. 68 Ge. However, if the distillation apparatus leaks, this method can lead to a large amount of [unclear - possibly related to a specific product or process]. 68 Ge product loss and potential radioactive contamination issues. Another method for separation is solvent extraction, which often uses organic reagents such as toluene or carbon tetrachloride as extractants for liquid-liquid extraction. However, to obtain FDA approval... 68 Ge / 68 Approval of Ga generator 68 The separation and purification process of Ge should use non-toxic and non-carcinogenic solvents. Furthermore, as mentioned earlier, germanium tetrachloride is a highly volatile species; therefore, achieving a higher radioactive concentration by reducing the volume of the product liquid through evaporation and concentration is not feasible. 68 Ge is impractical and may result in product evaporation and waste.

[0004] Existing technologies also employ the combined use of two resin columns for separation and purification. However, the acidity or alkalinity of the solution needs to be adjusted between the two resin columns (commonly known as adjusting the feed solution), making it impossible to achieve one-step separation and purification, resulting in low separation and purification efficiency. Summary of the Invention

[0005] Based on the above analysis, the present invention aims to provide a method for separation and purification using a combination of gel resin and cationic resin. 68 Ge's method is used to solve the problem that existing separation and purification methods cannot achieve one-step separation and purification, resulting in low separation and purification efficiency.

[0006] The objective of this invention is mainly achieved through the following technical solutions:

[0007] On the one hand, the present invention provides a method for separation and purification using a combination of gel resin and cationic resin.68 Ge's method includes the following steps:

[0008] Step (a): Dissolve and leach the gallium target after it has been irradiated by the accelerator to obtain a liquid solution;

[0009] Step (b): Adjust the pH of the feed solution to be alkaline;

[0010] Step (c): Pass the alkaline solution through a gel resin column.

[0011] Step (d): Elution of the gel resin column;

[0012] Step (e): [The text abruptly ends here, likely due to an incomplete sentence or a formatting error.] 68 The eluent of Ge was passed through a cation exchange resin column and washed to obtain... 68 Ge eluent.

[0013] Furthermore, the filler of the gel resin column is dextran gel resin.

[0014] Furthermore, the filler of the cation resin column is a strongly acidic cation resin.

[0015] Furthermore, in step (b), sodium hydroxide solution is used to adjust the feed solution to be alkaline.

[0016] Furthermore, sodium citrate solution is added in step (b).

[0017] Furthermore, the dextran gel resin is of the fine particulate type.

[0018] Furthermore, the strongly acidic cationic resin is macroporous.

[0019] Furthermore, the pH value of the feed solution in step (b) is 11-14.

[0020] Furthermore, the concentration of the sodium citrate solution is 1 mol / L.

[0021] On the other hand, the present invention also provides an application of the above-described method in the preparation of radiopharmaceuticals.

[0022] Compared with the prior art, the present invention can achieve at least one of the following beneficial effects:

[0023] (1) This invention achieves one-step separation and purification of the feed solution through a combination of raw material source selection, adjustment of the feed solution's acidity / alkalinity, and the use of a specific eluent, thereby improving separation and purification efficiency. Specifically, based on a specific raw material source (a gallium target irradiated by an accelerator), this invention specifically designs a method for separation and purification using a combination of gel resin columns and cation exchange resin columns. 68 Ge, and by adjusting the liquid to be alkaline, 68Ge in a specific soluble form 68 GeO(OH)3 - and 68 GeO2(OH)2 2- The sample is specifically adsorbed onto the gel resin column. Since the soluble form can be eluted with an acidic solution, and the cation exchange resin column functions optimally under acidic conditions, no preparation of the feed solution is required between the two resin columns, achieving one-step separation and purification of the feed solution, thereby improving separation and purification efficiency. Specifically, the separation and purification method of this invention can complete the entire separation and purification of 50 ml of feed solution in 100 minutes, while existing methods requiring intermediate preparation of the feed solution take approximately 200 minutes, with a separation and purification efficiency only half that of this invention.

[0024] (2) This invention improves the concentration of solvents in the feed solution by adding dissolving and leaching agents (hydrochloric acid and hydrogen peroxide) in batches. 68 The Ge content was reduced, while the content of Ga and other metal impurities in the feed solution was decreased, thereby improving the product's... 68 The recovery rate and purity of Ge (Ga removal rate of 99.99998%, close to 100%; Zn removal rate of 99.965%; Co removal rate of 99.9992%). Specifically, while meeting the requirements of the U.S. Department of Energy regarding radioactive concentration, the product of this invention... 68 Ge recovery rate is as high as 89%.

[0025] (3) Since the separation and purification method of the present invention does not use toxic and carcinogenic organic solvents, it complies with FDA requirements. 68 The separation and purification process of Ge should use non-toxic and non-carcinogenic solvents.

[0026] (4) The dextran gel resin column used in this invention requires no further treatment and can be directly recycled at least three times with its separation performance remaining essentially unchanged. The strongly acidic cation exchange resin can be regenerated sequentially using hydrochloric acid, sodium hydroxide, hydrochloric acid, and deionized water for reuse. Therefore, this invention establishes a recyclable dextran gel resin coupled with a cation exchange resin column for separation and purification. The process is simple to operate, easily automated, and can achieve… 68 Continuous and large-scale production of Ge products.

[0027] (5) In the method of the present invention, the two resin columns are connected in a specific order, namely, the gel resin column is in front and the cation resin column is behind, which not only improves the separation and purification effect, but also reduces the cost (because if the cation resin column is in front, the cation resin will be deactivated quickly).

[0028] (6) On the other hand, the separation and purification method of the present invention, through the combined adjustment of raw material source, pH adjustment of feed solution and use of specific eluent, enables the use of gel resin column and cation resin column with very small bed volume (2-4 mL) to meet the separation and purification requirements.

[0029] In this invention, the above-described technical solutions can be combined with each other to achieve more preferred combinations. Other features and advantages of this invention will be set forth in the following description, and some advantages will become apparent from the description or may be learned by practicing the invention. Attached Figure Description

[0030] The accompanying drawings are for illustrative purposes only and are not intended to limit the invention. Throughout the drawings, the same reference numerals denote the same parts.

[0031] Figure 1 In this embodiment of the invention, a series of gel resin and cation exchange resin columns are used for separation and purification. 68 Ge's process flow diagram;

[0032] Figure 2 The ion content in the effluent and washing liquid of the cation exchange resin column in Example 1. Detailed Implementation

[0033] The preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings, which constitute a part of the present invention and are used together with the embodiments of the present invention to illustrate the principles of the present invention, but are not intended to limit the scope of the present invention.

[0034] A specific embodiment of the present invention discloses a radiochemical separation and purification method. 68 Ge's method is used to separate and purify solutions obtained from accelerator-irradiated gallium targets. 68 The accelerator-irradiated gallium target includes 1 g of Ga, 500 μg of Zn, 500 μg of Co, and 600 μg of Ge.

[0035] Overall, the method of this invention is based on the specific adsorption of Ge by dextran gel resin under alkaline conditions to remove large amounts of Ga and metal impurities. 68 The separation of Ge. 68 The column adsorption stage of Ge. 68 Ge in soluble form 68 GeO(OH)3 - and 68 GeO2(OH)2 2- Gallium is specifically adsorbed in the gel resin column, while most gallium and other metal impurities elute through the gel resin column. Subsequently, hydrochloric acid solution is used to pass the gallium through the gel resin column... 68Ge desorption yields a product containing... 68 Ge eluent. Finally, the eluent containing... 68 The Ge eluent is directly purified of the remaining metal impurities using a cation exchange resin. Because this invention does not use organic solvents as extraction agents, the final product... 68 Ge contains virtually no organic or metallic impurities, and different radioactive concentrations can be obtained through process control. 68 Ge products are designed to meet market demands.

[0036] Specifically, before separation and purification, gel resin columns and cation exchange resin columns are prepared respectively.

[0037] In one embodiment, the gel resin column is prepared by the following method: weigh an appropriate amount of dry dextran gel resin and swell it in deionized water for 20-24 hours, then transfer the swollen gel resin to a chromatography column for sedimentation to obtain a gel resin column with a bed volume of about 2-4 mL.

[0038] In one embodiment, the strongly acidic cation exchange resin column is prepared by the following method:

[0039] Weigh an appropriate amount of dry cation exchange resin and soak it in 1 mol / L hydrochloric acid solution for 1-3 hours. Then, treat it sequentially with 1 mol / L sodium hydroxide solution, 1 mol / L hydrochloric acid solution, and deionized water for 1-3 hours to obtain pretreated cation exchange resin. Next, transfer the pretreated cation exchange resin to a chromatography column for precipitation to obtain a cation exchange resin column with a bed volume of 2-4 mL.

[0040] After preparing the gel resin column and the cation resin column, a peristaltic pump tube was used to connect the eluent outlet of the gel resin column to the injection end of the cation resin column to obtain a gel resin and a cation resin tandem resin column.

[0041] The following is combined Figure 1 This paper introduces the separation and purification of gel resin and cation exchange resin in series using the above method. 68 Ge's method includes the following steps:

[0042] Step (a): The gallium target irradiated by the accelerator is dissolved and leached to obtain a solution. This step specifically includes the following steps:

[0043] Step a1: Cool the gallium target after it has been irradiated by the accelerator for two weeks, then pour the gallium target into a melter and heat it to a certain temperature in a water bath to melt the gallium.

[0044] Step a2: Add the dissolving and leaching agent in batches, stirring to obtain a solution containing metallic impurities. Specifically, the dissolving and leaching agent is a mixed solution of hydrochloric acid of a certain concentration and hydrogen peroxide of a certain mass percentage concentration.

[0045] In one embodiment, the concentration of hydrochloric acid is 2-6 mol / L. For example, the concentration of hydrochloric acid can be 2 mol / L, 2.5 mol / L, 3 mol / L, 3.5 mol / L, 4 mol / L, 4.5 mol / L, 5 mol / L, 5.5 mol / L, or 6 mol / L.

[0046] In one embodiment, the mass percentage concentration of hydrogen peroxide is 10%-40%. For example, 10%, 15%, 20%, 25%, 30%, 35%, and 40%.

[0047] In one embodiment, the water bath temperature is between 40-60°C. For example, 40°C, 43°C, 45°C, 47°C, 50°C, 52°C, 55°C, 58°C, and 60°C.

[0048] In one embodiment, the stirring time in step a2 is 30 min to 1 hour. For example, 30 min, 35 min, 40 min, 50 min, 55 min, or 60 min.

[0049] The solution obtained by dissolving the irradiated gallium target in step (a) is a clear and transparent solution, which contains at least [missing information - likely a specific ingredient or component]. 68 Ge, Ga, Zn, Co, etc.

[0050] Step (b): Filter the liquid and then adjust the pH of the liquid to be alkaline.

[0051] In one embodiment, sodium citrate solution is added first, followed by sodium hydroxide solution to adjust the pH value of the solution.

[0052] The purpose of adding sodium citrate solution is twofold: first, to allow metallic impurities in the solution to complex with citrate ions and dissolve in the solution, thus preventing precipitation; and second, to maintain a stable pH value in the solution.

[0053] In one embodiment, the pH value of the adjusted feed solution is 11-14, for example, pH values ​​of 11, 12, 13, and 14.

[0054] Step (c): Pass the alkaline solution obtained in step (b) through a gel resin column at a flow rate of 1 mL / min.

[0055] It should be noted that in step (c), 68 Ge will be in soluble form 68 GeO(OH)3 - and 68 GeO2(OH)2 2- It exists and is specifically adsorbed in the gel resin column, while most metal impurities such as Ga, Zn, and Co will flow out through the gel resin column.

[0056] Step (d): Elute the gel resin column with a certain volume of 0.05-0.5 mol / L hydrochloric acid solution, and elute the gel resin column adsorbed in step (b). 68 Ge was desorbed to achieve preliminary separation. 68 Ge eluent.

[0057] In one embodiment, the gel resin column is packed with fine-particle dextran gel resin. Specifically, the particle size of the dextran gel resin is between 20-80 μm. Using fine-particle gel resin results in a larger adsorption capacity for Ge and better separation performance.

[0058] Between steps (c) and (d) is washing the gel resin column. Specifically, the gel resin column is washed with a sodium citrate solution of a specific pH value. Some metallic impurities are quantitatively washed out. The column is then further washed with a specific volume of deionized water to prepare it for subsequent treatment with hydrochloric acid solution. 68 Ge was used for elution.

[0059] In one embodiment, the pH value of the sodium citrate solution used to wash the gel resin column is the same as the pH value of the feed solution in step (b). The purpose is that, on the one hand, under this condition, Ga complexes with sodium citrate, which facilitates the washing off of Ga adhering to the resin or glass column; on the other hand, after the feed solution passes through the gel resin column, some impurities such as Ga may not flow out completely and adhere to the resin column, so washing is required.

[0060] Step (e): The contents obtained in step (d) 68 The eluent for Ge was passed through a cation exchange resin column. 68 Therefore 68 Ge(OH)4 is collected directly through the cation exchange resin, while metal impurities are retained almost quantitatively in cationic form.

[0061] In one embodiment, the cation exchange resin column is filled with a macroporous, strongly acidic cation exchange resin. Specifically, the pore size of the cation exchange resin is between 100 and 200 mesh. Macroporous, strongly acidic cation exchange resins have a strong adsorption capacity for metallic impurities, and also have a high adsorption capacity, thus allowing them to be used multiple times before deactivation.

[0062] In one embodiment, AG MP-50 strong acid cation exchange resin and AG50WX8 strong acid cation exchange resin from Bio-Rad were used. Results showed that using AG MP-50 cation exchange resin was more effective than using AG 50WX8 cation exchange resin. 68 Ge has a higher recovery rate.

[0063] Using the above separation and purification method, under the premise of meeting the U.S. Department of Energy's requirements for radioactivity concentration, the obtained product contains... 68 The recovery rate of Ge is as high as 89%, and the removal rate of metal impurities is also high. For example, the removal rate of Ga is 99.99998%, close to 100%; the removal rate of Zn is 99.965%; and the removal rate of Co is 99.9992%.

[0064] Example 1

[0065] Step 1: After accelerator irradiation, the gallium target is cooled for two weeks. Then, the gallium target is poured into a dissolver, and the dissolver is heated in a water bath. The water bath temperature is raised to 45°C to melt the gallium.

[0066] Step 2: Add 8 mL of a mixed solution of 4 mol / L hydrochloric acid and 1 mL of 30% hydrogen peroxide to the dissolver. Finally, add a small magnetic stir bar and turn on the stirrer. Maintain the water bath temperature at 45°C for the dissolution and leaching experiment. Stir for 1 hour, then turn off the magnetic stirrer and water bath heating. Pour out the leachate and collect it.

[0067] Repeat step 2 four times to obtain approximately 45 mL of liquid.

[0068] Experimental results: The final gallium content in the 45mL solution was approximately 1g. The reaction was relatively mild throughout the experiment.

[0069] Step 3: First add sodium citrate solution, then add sodium hydroxide solution to adjust the pH of the solution to 13, with the citrate concentration at around 1 mol / L.

[0070] Step 4: Pass the pH-adjusted solution through a dextran gel resin column at a flow rate of 1 mL / min. Most of the matrix element gallium and metal impurities are removed by flowing out through the gel resin.

[0071] The gel resin column was then washed with a sodium citrate solution at pH 13 for 10 bed volumes. This washing step removed almost all remaining gallium matrix elements and metallic impurities. The column was then washed again with one bed volume of deionized water to prepare for subsequent hydrochloric acid elution of Ge.

[0072] Step 5: Use 0.25 mol / L hydrochloric acid solution to elute Ge adsorbed on the gel resin. Elute for 5 bed volumes. Pass the eluent through a cation exchange resin column at a controlled flow rate. Ge flows directly through the cation exchange resin as Ge(OH)4 and is collected, while the metal impurity cations are almost quantitatively retained. Finally, wash the cation exchange resin column with 0.25 mol / L hydrochloric acid solution for 1.5 bed volumes. Collect all effluent and washings. The trend of metal content in the effluent and washings with elution column volume is shown below. Figure 2As shown.

[0073] In this embodiment, the gel resin column is filled with Sephadex G-25 gel resin from Sigma Reagents; the cation resin column is filled with AG MP-50 strong acidic cation resin from Bio-Rad.

[0074] In this embodiment, ICP-MS was used to analyze the metal content in the feed solution and the Ge-containing eluent after separation and purification. The experimental results are shown in Table 1.

[0075] Table 1. Metal content in the feed solution and the Ge-containing eluent after separation and purification.

[0076]

[0077] As shown in Table 1, the Ge-containing eluent obtained using the separation and purification method of this embodiment, under the premise of meeting the US Department of Energy specifications (requiring a radioactive concentration greater than 50 mCi / mL), yields a product with... 68 The amount of Ge was 537 μg, with a recovery rate of 89%. Furthermore, the amounts of other metals in the washing solution were very low. Specifically, the amount of Ga was only 0.17 μg, with a removal rate of 99.99998%, close to 100%; the amount of Zn was only 0.20 μg, with a removal rate of 99.6%; and the amount of Co was only 0.003 μg, with a removal rate of 99.999%. Therefore, this embodiment achieved [the desired level of recovery]. 68 Ge can be separated and purified in one step (no acid or alkalinity adjustment is required between the two resin columns), and the target product recovery rate and impurity metal removal rate are high.

[0078] Example 2

[0079] This embodiment is similar to Embodiment 1, except that the water bath temperature in steps 1 and 2 is 60°C; the concentration of hydrochloric acid in step 2 is 6 mol / L and the stirring time is 30 min; the pH value in step 3 is 12.5; and the pH value of the sodium citrate solution used to wash the gel resin column in step 4 is 12.5.

[0080] The metal content in the feed solution and the Ge-containing eluent after separation and purification was also analyzed using ICP-MS. The experimental results are shown in Table 2.

[0081] Table 2. Metal content in the feed solution and the Ge-containing eluent after separation and purification.

[0082]

[0083] As shown in Table 2, the Ge-containing eluent obtained using the separation and purification method of this embodiment, under the premise of meeting the European Pharmacopoeia's requirements for radioactivity concentration, yields a product with... 68The amount of Ge was 524 μg, with a recovery rate of 87%. Furthermore, the amounts of other metals in the washing solution were very low. Specifically, the amount of Ga was only 0.19 μg, with a removal rate of 99.99998%, close to 100%; the amount of Zn was only 0.18 μg, with a removal rate of 99.965%; and the amount of Co was only 0.004 μg, with a removal rate of 99.9992%. Therefore, this embodiment achieved [the desired level of recovery]. 68 Ge can be separated and purified in one step (no acid or alkalinity adjustment is required between the two resin columns), and the target product recovery rate and impurity metal removal rate are high.

[0084] Example 3

[0085] This embodiment is similar to Embodiment 1, except that the water bath temperature in steps 1 and 2 is 40°C; the concentration of hydrochloric acid in step 2 is 2 mol / L and the stirring time is 45 min; the pH value in step 3 is 13.5; and the pH value of the sodium citrate solution used to wash the gel resin column in step 4 is 13.5.

[0086] The metal content in the feed solution and the Ge-containing eluent after separation and purification was also analyzed using ICP-MS. The experimental results are shown in Table 3.

[0087] Table 3. Metal content in the feed solution and the Ge-containing eluent after separation and purification.

[0088]

[0089] As shown in Table 3, the Ge-containing eluent obtained using the separation and purification method of this embodiment, under the premise of meeting the European Pharmacopoeia's requirements for radioactivity concentration, yields a product with... 68 The amount of Ge was 528 μg, with a recovery rate of 88%. Furthermore, the amounts of other metals in the washing solution were very low. Specifically, the amount of Ga was only 0.19 μg, with a removal rate of 99.99998%, close to 100%; the amount of Zn was only 0.18 μg, with a removal rate of 99.965%; and the amount of Co was only 0.004 μg, with a removal rate of 99.9992%. Therefore, this embodiment achieved [the desired level of recovery]. 68 Ge can be separated and purified in one step (no acid or alkalinity adjustment is required between the two resin columns), and the target product recovery rate and impurity metal removal rate are high.

[0090] Comparative Example 1

[0091] This embodiment is similar to Embodiment 1, except that in step 5, 0.25 mol / L hydrochloric acid solution is used to elute 10 bed volumes.

[0092] The metal content in the feed solution and the Ge-containing eluent after separation and purification was also analyzed using ICP-MS. The experimental results are shown in Table 4.

[0093] Table 4. Metal content in the feed solution and the Ge-containing eluent after separation and purification.

[0094]

[0095] As can be seen from Table 4, when the volume of the eluent is increased, 68 Ge recovery rates can reach up to 99.5%. However, the radioactivity concentration of the eluent is 30 mCi / mL, which does not meet the requirements of the U.S. Department of Energy regarding radioactivity concentration.

[0096] Comparative Example 2

[0097] This embodiment is similar to Embodiment 1, except that the hydrochloric acid and hydrogen peroxide mixture is added all at once, not in batches. Specifically, 40 mL of 4 mol / L hydrochloric acid and 5 mL of 30% hydrogen peroxide mixture are added all at once.

[0098] Violent reaction occurred during the experiment, and the temperature of the reaction system rose rapidly. It was difficult to control the temperature in the water bath. The increase in reaction temperature would exacerbate the dissolution of metallic gallium. On the other hand, the boiling point of germanium chloride is very low, only 84°C, which may cause product volatilization loss.

[0099] The metal content in the feed solution and the Ge-containing eluent after separation and purification was also analyzed using ICP-MS. The experimental results are shown in Table 5.

[0100] Table 5. Metal content in the feed solution and the Ge-containing eluent after separation and purification.

[0101]

[0102] As shown in Table 5, adding a mixed solution of hydrochloric acid and hydrogen peroxide in one step causes a rapid increase in the reaction system temperature, exacerbating the dissolution of metallic gallium and significantly increasing the amount of Ga in the solution to 2,564,739 μg, thus increasing the difficulty of subsequent processing. Furthermore... 68 The recovery rate of Ge was only 75.8%.

[0103] Comparative Example 3

[0104] This embodiment is similar to Example 1, except that the cation exchange resin column is filled with AG 50WX8 strong acid cation exchange resin from Bio-Rad. Results show that... 68 The recovery rate of Ge was only 76%, and the removal rate of metal impurities was similar to that of AG MP-50 strong acid cation exchange resin.

[0105] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any changes or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for separating and purifying a gel resin and a cation resin in combination 68 The method of Ge is characterized in that, The method is: Step (a): dissolving and leaching the metal gallium target after accelerator irradiation to obtain a feed liquid; Step (b): filtering the feed liquid, first adding a sodium citrate solution, and then adding a sodium hydroxide solution to adjust the pH value of the feed liquid to 11-14; Step (c): passing the alkaline feed solution through a gel resin column, 68 Ge in soluble form 68 GeO(OH)3 - and 68 GeO2(OH)2 2- specifically adsorbed in the gel resin column, after which the gel resin column is washed with a sodium citrate solution having the same pH as the feed solution in step (b), followed by continued washing of the gel resin column using deionized water, so that Ge is subsequently eluted using a hydrochloric acid solution; 68 Ge Step (d): eluting the gel resin column with a 0.05-0.5 mol / L concentration of hydrochloric acid solution, and the filler of the gel resin column is a fine particle type dextran gel resin with a particle size of 20-80 μm; Step (e): The Ge eluate was washed through a column of macroporous strong acid cation resin with a pore size between 100-200 mesh to obtain 68 Ge eluate; and 68 Ge eluate; and Step (a) comprises the following steps: Step a1: cooling the metal gallium target after accelerator irradiation for two weeks, then pouring the metal gallium target into a dissolver, and heating to 40-60°C under water bath conditions to melt the metal gallium; Step a2: adding the dissolving leaching agent in batches, stirring for 30 min-1 hour to obtain a feed liquid; The dissolving leaching agent is a mixed solution of hydrochloric acid with a concentration of 2-6 mol / L and hydrogen peroxide with a mass percentage concentration of 10%-40%.

2. The method of claim 1, wherein, The concentration of the sodium citrate solution is 1 mol / L.

3. Use of the method of claim 1 or 2 in the preparation of a radiopharmaceutical.

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