Processing technology of calcined Magnetitum based on concept of QbD and its XRD characteristic spectra.
10.19540/j.cnki.cjcmm.20250218.301
- Author:
De-Wen ZENG
1
;
Jing-Wei ZHOU
1
;
Tian-Xing HE
1
;
Yu-Mei CHEN
2
;
Huan-Huan XU
1
;
Jian FENG
2
;
Yue YANG
1
;
Xin CHEN
1
;
Jia-Liang ZOU
1
;
Lin CHEN
1
;
Hong-Ping CHEN
1
;
Shi-Lin CHEN
1
;
Yuan HU
1
;
You-Ping LIU
1
Author Information
1. State Key Laboratory of Southwestern Chinese Medicine Resources, School of Pharmacy,Chengdu University of Traditional Chinese Medicine Chengdu 611137, China.
2. Sichuan New Green Pharmaceutical Technology Development Co., Ltd. Pengzhou 611930, China.
- Publication Type:Evaluation Study
- Keywords:
AHP-CRITIC hybrid weighting method;
Magnetitum;
X-ray diffraction method;
XRD characteristic spectra;
mineral medicine;
processing techno-logy;
quality by design(QbD)
- MeSH:
X-Ray Diffraction/methods*;
Drugs, Chinese Herbal/chemistry*;
Quality Control;
Particle Size
- From:
China Journal of Chinese Materia Medica
2025;50(9):2391-2403
- CountryChina
- Language:Chinese
-
Abstract:
Guided by the concept of quality by design(QbD), this study optimizes the calcination and quenching process of calcined Magnetitum and establishes the XRD characteristic spectra of calcined Magnetitum, providing a scientific basis for the formulation of quality standards. Based on the processing methods and quality requirements of Magnetitum in the Chinese Pharmacopoeia, the critical process parameters(CPPs) identified were calcination temperature, calcination time, particle size, laying thickness, and the number of vinegar quenching cycles. The critical quality attributes(CQAs) included Fe mass fraction, Fe~(2+) dissolution, and surface color. The weight coefficients were determined by combining Analytic Hierarchy Process(AHP) and the criteria importance though intercrieria correlation(CRITIC) method, and the calcination process was optimized using orthogonal experimentation. Surface color was selected as a CQA, and based on the principle of color value, the surface color of calcined Magnetitum was objectively quantified. The vinegar quenching process was then optimized to determine the best processing conditions. X-ray diffraction(XRD) was used to establish the characteristic spectra of calcined Magnetitum, and methods such as similarity evaluation, cluster analysis, and orthogonal partial least squares-discriminant analysis(OPLS-DA) were used to evaluate the quality of the spectra. The optimized calcined Magnetitum preparation process was found to be calcination at 750 ℃ for 1 h, with a laying thickness of 4 cm, a particle size of 0.4-0.8 cm, and one vinegar quenching cycle(Magnetitum-vinegar ratio 10∶3), which was stable and feasible. The XRD characteristic spectra analysis method, featuring 9 common peaks as fingerprint information, was established. The average correlation coefficient ranged from 0.839 5-0.988 1, and the average angle cosine ranged from 0.914 4 to 0.995 6, indicating good similarity. Cluster analysis results showed that Magnetitum and calcined Magnetitum could be grouped together, with similar compositions. OPLS-DA discriminant analysis identified three key characteristic peaks, with Fe_2O_3 being the distinguishing component between the two. The final optimized processing method is stable and feasible, and the XRD characteristic spectra of calcined Magnetitum was initially established, providing a reference for subsequent quality control and the formulation of quality standards for calcined Magnetitum.
