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| Determination of Aluminum in Vaccines by Monochromatic
Excitation-Energy Dispersive X-Ray Fluorescence Spectrometry |
| LIU Cong-cong1, 2, WEN Jia-xin1, 3*, LIN Yuan-heng1, 2, LIANG Wei-yang1, 2, YANG Zhi-ye1, 3, DENG Feng1, 3, LUO Xin-yang4, ZHAO Miao-miao5 |
1. Guangdong Institute for Drug Control, Guangzhou 510663, China
2. NMPA Key Laboratory for Quality Control of Blood Products, Guangzhou 510663, China
3. NMPA Key Laboratory for Rapid Testing Technology of Drugs, Guangzhou 510663, China
4. RayKol Group Corp., Ltd., Xiamen 361000, China
5. Suzhou Jiapu Technology Limited Company, Suzhou 215000, China
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Abstract The aluminum adjuvant content in vaccines is an important factor affecting the effectiveness and safety of vaccines. Determining the aluminum content in vaccines swiftly and accurately is an urgent requirement for both production enterprises and inspection institutions. In this paper, the monochromatic excitation technology of a doubly curved crystal was applied to energy dispersive X-ray fluorescence spectrometry, and the matrix effect was corrected by the fundamental parameter method. Samples were pretreated by heating in 30% nitric acid solution at 40 ℃ for 25 minutes. A polypropylene film with a thickness of 4 μm was used as the backing material. Detection was carried out for 300 seconds under the excitation conditions of low voltage and high current, and an analytical method for rapidly determining the aluminum content in vaccines was established. The results showed a significant positive correlation between the measured and theoretical values of aluminum in six vaccine matrices. The correlation coefficients of the fitting equations were all greater than 0.998. The detection limit and quantification limit of the method were 0.027 and 0.090 mg·mL-1, respectively. Within spiking levels ranging from 0.3 to 0.7 mg·mL-1, average recovery rates fell between 97.6% and 102%, with precision RSD (n=6) recorded at 2.4% to 6.7%. The coefficient of variation for the same sample measured within 90 days was 4.7%. The accuracy was verified with ICP-OES and ICP-MS as references. The results of 70 batches of vaccine products of six varieties showed good consistency with the reference values, and the absolute values of relative errors did not exceed 10%. This method enables on-site testing without reliance on precision equipment while maintaining accuracy. The research indicates that using monochromatic excitation-energy dispersive X-ray fluorescence spectroscopy offers several advantages, including eliminating the need for standard materials, high accuracy, good precision, and a low detection limit. This technique is suitable for rapid on-site determination of aluminum content in vaccines and holds broad practical significance for widespread application.
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Received: 2024-12-05
Accepted: 2025-04-15
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Corresponding Authors:
WEN Jia-xin
E-mail: ellawen224@qq.com
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