加速器生产医用同位素211At及单抗标记

doi:10.6023/A21060266

化学学报 ›› 2021, Vol. 79 ›› Issue (11): 1376-1384.DOI: 10.6023/A21060266 上一篇下一篇

研究论文

加速器生产医用同位素²¹¹At及单抗标记

陈德胜^a^,^b^,^d, 刘葳豪^c, 黄清钢^a^,^b, 曹石巍^a^,^b, 田伟^a^,^b, 殷小杰^a^,^b, 谈存敏^a^,^b, 王洁茹^a^,^b^,^d^,^e, 初剑^a^,^d, 贾子萌^a^,^d, 程念炜^e, 高瑞勤^a^,^b, 吴晓蕾^a^,^b, 秦芝^a^,^b^,^*(), 范芳丽^a^,^b, 白静^a^,^b, 李飞泽^c, 廖家莉^c, 杨远友^c, 刘宁^c

a 中国科学院近代物理研究所兰州 730000
b 先进能源科学与技术广东省实验室惠州 516000
c 四川大学原子核科学技术研究所辐射物理及技术教育部重点实验室成都 610064
d 中国科学院大学核科学与技术学院北京 100049
e 兰州大学核科学与技术学院兰州 730000

投稿日期:2021-06-11 发布日期:2021-08-17
通讯作者: 秦芝
基金资助:
甘肃省引导科技创新发展专项资金资助项目

Accelerator Production of the Medical Isotope ²¹¹At and Monoclonal Antibody Labeling

Desheng Chen^a^,^b^,^d, Weihao Liu^c, Qinggang Huang^a^,^b, Shiwei Cao^a^,^b, Wei Tian^a^,^b, Xiaojie Yin^a^,^b, Cunmin Tan^a^,^b, Jieru Wang^a^,^b^,^d^,^e, Jian Chu^a^,^d, Zimeng Jia^a^,^d, Nianwei Cheng^e, Ruiqin Gao^a^,^b, Xiaolei Wu^a^,^b, Zhi Qin^a^,^b(), Fangli Fan^a^,^b, Jing Bai^a^,^b, Feize Li^c, Jiali Liao^c, Yuanyou Yang^c, Ning Liu^c

a Institute of Modern Physics, Chinese Academy of Sciences, Lanzhou 730000, China
b Advanced Energy Science and Technology Guangdong Laboratory, Huizhou 516000, China
c Key Laboratory of Radiation Physics and Technology, Ministry of Education, Institute of Nuclear Science and Technology, Sichuan University, Chengdu 610064, China
d School of Nuclear Science and Technology, University of Chinese Academy of Sciences, Beijing 100049, China
e School of Nuclear Science and Technology, Lanzhou University, Lanzhou 730000, China

Received:2021-06-11 Published:2021-08-17
Contact: Zhi Qin
Supported by:
Special Fund for Scientific and Technological Innovation and Development of Gansu Province of China

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摘要/Abstract

²¹¹At, 半衰期7.2 h, 发射的α粒子具有很高的线性传能密度, 是一种理想的靶向α治疗核素. 利用中国科学院近代物理研究所强流超导直线加速器提供的α束流辐照Bi靶生产²¹¹At, 系统考察了加速器生产²¹¹At的整个流程, 包括加速器辐照、干蒸馏分离、质量分析以及单抗标记. 研究结果表明, 干蒸馏分离²¹¹At的总收率最高达78.53%, 获得的固体²¹¹At产品具有极高的比活度、核纯度以及化学纯度, 其中杂质元素Bi、Cu、Zn、Al含量均低于100 ng/GBq, 且入射粒子能量低于28.2 MeV时, N(²¹⁰At)/N(²¹¹At)值低于10^–5, 研究也实现了²¹¹At在尼妥珠单抗上的标记, 标记率高达94.86%. 基于以上研究我们确立了一套简单、高效的分离方法, 为后续我国²¹¹At的生产和应用奠定了良好基础.

关键词: 加速器, 医用同位素, 干蒸馏法, ²¹¹At, 标记

²¹¹At, with a half-life of 7.2 h, is an excellent radionuclide being investigated for use in targeted alpha therapy as the result of very high linear energy transfer. However, the production of ²¹¹At is limited by ²¹⁰At, because ²¹⁰At decays to produce long half-life (138.4 d) extremely toxic daughter ²¹⁰Po. The production of ²¹¹At via ²⁰⁹Bi(α,2n) nuclear reaction and ²¹⁰At via ²⁰⁹Bi(α,3n) nuclear reaction, as the energy of incident α-particle increases, the ratio of N(²¹⁰At)/N(²¹¹At) increases. In this research, the α-particle is provided by the Chinese Accelerator Driven Sub-critical System (ADS) Front-end Demo Linac at Institute of Modern Physics, Chinese Academy of Sciences. The technical process of ²¹¹At produced was studied systematically, including accelerator irradiation, separation by dry distillation method, quality analysis, and monoclonal antibody labeling. The bismuth targets were irradiated with α-particle by 28.18, 28.34, 28.48 28.92 MeV, and the target chamber adopts an inclined target with water cooling to improve the cooling effect. The dry distillation separation was carried out at a high temperature of 850 ℃, oxygen as the carrier gas, chloroform and ethanol as eluent, and the chloroform solution containing ²¹¹At was blow dry with nitrogen. The results showed that the total recovery of dry distillation separation of ²¹¹At reached 78.53%. After separation, the quality analysis of ²¹¹At was performed using a high-purity Ge-detector, alpha energy spectrometer, and mass spectrometer. The obtained solid ²¹¹At had high specific activity, radionuclide purity and chemical purity, where the content of impurity elements Bi, Cu, Zn, and Al was less than 100 ng/GBq, and the ratio of N(²¹⁰At)/N(²¹¹At) was less than 10^–5 when the incident particle energy is below 28.2 MeV. Finally, the labeling of ²¹¹At-nimotuzumab was realized through N-succinimidyl-3-(trimethylstannyl)benzoate, and the labeling rate was 94.86%. Based on this research, a set of simple and efficient separation methods was established, which laid a good foundation for the subsequent production and application of ²¹¹At in China.

Key words: accelerator, medical isotope, dry distillation method, ²¹¹At, labeling

引用此文

陈德胜, 刘葳豪, 黄清钢, 曹石巍, 田伟, 殷小杰, 谈存敏, 王洁茹, 初剑, 贾子萌, 程念炜, 高瑞勤, 吴晓蕾, 秦芝, 范芳丽, 白静, 李飞泽, 廖家莉, 杨远友, 刘宁. 加速器生产医用同位素²¹¹At及单抗标记[J]. 化学学报, 2021, 79(11): 1376-1384.

Desheng Chen, Weihao Liu, Qinggang Huang, Shiwei Cao, Wei Tian, Xiaojie Yin, Cunmin Tan, Jieru Wang, Jian Chu, Zimeng Jia, Nianwei Cheng, Ruiqin Gao, Xiaolei Wu, Zhi Qin, Fangli Fan, Jing Bai, Feize Li, Jiali Liao, Yuanyou Yang, Ning Liu. Accelerator Production of the Medical Isotope ²¹¹At and Monoclonal Antibody Labeling[J]. Acta Chimica Sinica, 2021, 79(11): 1376-1384.

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图/表 20

图1. 209Bi(α,xn)210-211At反应的激发函数

Figure 1. The excitation function of 209Bi(α, xn)210-211At reaction

图2. 211At和210At衰变链

Figure 2. The decay chains of 211At and 210At

靶材料	Bi-209	Bi-209	Bi-209	Bi-209
束流能量(MeV)	30.10	30.65	29.90	29.60
打靶数量	7	1	2	1
能损^a(MeV)/碳膜窗(40 μm)	1.42	1.40	1.42	1.42
能损^a(MeV)/冷却氦气 1.25 atm (65 mm)	0.34	0.33	0^b	0^a
剩余能量(MeV)	28.34	28.92	28.48	28.18
束流与靶面夹角(°)	15	15	15	15

表1. 靶辐照参数(一)

Table 1. The irradiation parameters (Part 1)

序号	靶厚/(mg•cm^–2)	入射能量/MeV	平均流强/μA	辐照时间/h	EOB活度/MBq
序号	靶厚/(mg•cm^–2)	入射能量/MeV	平均流强/μA	辐照时间/h	理论值	实测值
1	10.18	28.34	1.88	1.20	45.97	43.83±4.26
2	13.83	28.34	2.03	1.03	50.57	41.98±3.62
3	15.71	28.34	1.90	1.13	54.11	49.49±2.88
4	17.48	28.34	1.95	2.05	103.78	118.82±7.08
5	19.89	28.34	2.05	2.01	107.78	61.78±3.63
6	15.43	28.34	1.85	2.26	105.69	109.89±6.34
7	9.97	28.34	2.07	2.04	83.91	85.97±4.96
8	10.18	28.92	2.05	1.50	76.31	88.83±5.16
9	19.07	28.48	7.07	1.83	344.97	73.36±1.81
10	18.55	28.48	8.18	4.08	889.78	314.61±3.47
11	19.05	28.18	10.02	4.08	993.87	351.18±4.12

表2. 靶辐照参数(二)

Table 2. The irradiation parameters (Part 2)

图3. 辐照前(a)、第一轮辐照后(b)和第二轮辐照后(c)的Bi靶

Figure 3. The morphology of the Bi target before irradiation (a), after the first round of irradiation (b) and after the second round of irradiation (c)

图4. 211At厚靶产额随辐照时间变化趋势图

Figure 4. The tendency chart of the thick target yield of 211At with irradiation time

图5. 28.34 MeV和28.92 MeV的α束流辐照后Bi靶的γ能谱图

Figure 5. The γ spectra of irradiated Bi targets by α beam at 28.34 MeV and 28.92 MeV

图6. 辐照后的Bi靶经不同冷却时间后的γ能谱图(Eα=28.34 MeV)

Figure 6. The γ spectra of irradiated Bi targets with different cooling times

靶序号	温度/℃	气流量/(mL•min^–1)	保温时间/min	洗涤液	洗涤液用量(mL)			收集率
靶序号	温度/℃	气流量/(mL•min^–1)	保温时间/min	洗涤液	一段	二段	三段	一段	二段	三段
1	850	15	15	CHCl₃	0.4	2.0	—	—	—	—
2	850	15	15	CHCl₃	0.4	1.0	—	—	—	—
3	850	15	15	CHCl₃	5.0	10.0	—	—	—	—
4	850	15	15	CHCl₃	4.0	5.0	—	54.85±8.22%	1.42±8.35%	—
5	850	08	15	CHCl₃	1.0	5.0	—	34.40±8.29%	3.51±8.28%	—
6	850	10	15	CHCl₃	1.0	5.0	—	27.73±8.17%	2.48±8.17%	—
7	850	15	15	C₂H₆O	0.4	1.0	—	39.45±8.15%	5.14±8.17%	—
8	850	15	25	C₂H₆O	0.8	1.0	—	41.63±8.22%	3.37±8.29%	—
9	850	15	20	CHCl₃	0.4	0.4	—	42.83±5.60%	4.53±5.93%	—
10	850	15	20	CHCl₃	0.4	0.4	—	44.71±5.82%	17.44±6.30%	—
11	850	15	20	CHCl₃	0.4	0.4	1.0	48.69±5.79%	15.86±6.36%	13.98±6.43%

表3. 干蒸馏分离实验条件和结果

Table 3. The experimental conditions and results of dry distillation

图7. 211At产品液(0.4 mL)

Figure 7. The 211At product solution (0.4 mL)

种态	At	AtO₂	HAtO
–ΔH_ads/(kJ•mol^–1)	124±5	83±5	47±5
ΔH_subl/(kJ•mol^–1)	148±25	106±30	56±30

表4. At、AtO2和HAtO在石英表面的吸附焓(ΔHads)和升华焓(ΔHsubl)

Table 4. The adsorption enthalpy and sublimation enthalpy of astatine species on quartz surface

图8. HAtO在冷阱管中的热色谱沉积曲线的Monte Carlo模拟结果

Figure 8. Adsorption curves of thermochromatography for HAtO in the cold trap with Monte Carlo simulation

图9. 28.34 MeV和28.92 MeV辐照生产的211At产品γ能谱图

Figure 9. The γ spectra of 211At obtained at 28.34 MeV and 28.92 MeV

图10. 211At产品在不同冷却时间下的α能谱图

Figure 10. The α spectra of 211At with different cooling times

能量(MeV)	N(²¹⁰At)/N(²¹¹At)
能量(MeV)	α能谱法	γ能谱法
28.18	7.07×10^–6	<5.73×10^–7
28.34	1.61×10^–5	4.19×10^–6
28.48	4.35×10^–5	1.42×10^–5
28.92	3.05×10^–4	1.38×10^–4

表5. N(210At)/N(211At)的比值

Table 5. The ratio of N(210At)/N(211At)

图11. 一步法标记211At-ATE-nimotuzumab混合物的TLC分析

Figure 11. TLC analysis of 211At-ATE-nimotuzumab mixture labeled by one-step method

图12. 211At-ATE-nimotuzumab纯化物的TLC分析

Figure 12. TLC analysis of 211At-ATE-nimotuzumab after purification

t/h	PBS/%	FBS/%
3	94.25	87.34
6	92.73	86.42
12	85.71	76.71
24	79.31	73.87

表6. 211At-ATE-nimotuzumab放化纯在不同介质中随时间的变化

Table 6. Radiochemical purity change of 211At-ATE-nimotuzumab in different media

图13. 干蒸馏法分离211At的流程图

Figure 13. The flow chart for separation of 211At by dry distillation

图14. 干蒸馏分离211At的装置

Figure 14. The equipment used for dry distillation

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	( 林茂盛, 秦芝, 郭俊盛, 张丽娜, 丁华杰, 范芳丽, 白静, 雷富安, 吴晓蕾, 李小飞, 核化学与放射化学, 2009, 31, 28.)

加速器生产医用同位素²¹¹At及单抗标记

Accelerator Production of the Medical Isotope ²¹¹At and Monoclonal Antibody Labeling

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