Optimization of Processing Technology of Calcined Pyritum Based on QbD Concept and Its XRD Fingerprint Analysis
10.13422/j.cnki.syfjx.20250765
- VernacularTitle:基于QbD理念的煅自然铜炮制工艺优化及其XRD指纹图谱分析
- Author:
Xin CHEN
1
;
Jingwei ZHOU
1
;
Haiying GOU
1
;
Lei ZHONG
2
;
Tianxing HE
1
;
Wenbo FEI
2
;
Jialiang ZOU
1
;
Yue YANG
1
;
Dewen ZENG
1
;
Lin CHEN
1
;
Hongping CHEN
1
;
Shilin CHEN
1
;
Yuan HU
1
;
Youping LIU
1
Author Information
1. State Key Laboratory of Southwestern Traditional Chinese Medicine（TCM） Resources， School of Pharmacy，Chengdu University of TCM，Chengdu 611137，China
2. Sichuan Neo-green Pharmaceutical Technology Development Co. Ltd.，Pengzhou 611930，China
- Publication Type:Journal Article
- Keywords:
quality by design（QbD）;
Pyritum;
processing process;
differential thermal analysis;
X-ray diffraction（XRD）;
inductively coupled plasma mass spectrometry（ICP-MS）;
fingerprint
- From:
Chinese Journal of Experimental Traditional Medical Formulae
2025;31(13):197-205
- CountryChina
- Language:Chinese
-
Abstract:
ObjectiveBased on the concept of quality by design（QbD）， the processing process of calcined Pyritum was optimized， and its X-ray diffraction（XRD） fingerprint was established. MethodsThe safety， effectiveness and quality controllability of calcined Pyritum were taken as the quality profile（QTPP）， the color， hardness， metallic luster， phase composition， the contents of heavy metals and hazardous elements were taken as the critical quality attributes（CQAs）， and the calcination temperature， calcination time， paving thickness and particle size were determined as the critical process parameters（CPPs）. Differential thermal analysis， X-ray diffraction（XRD） and inductively coupled plasma mass spectrometry（ICP-MS） were used to analyze the correlation between the calcination temperature and CQAs of calcined Pyritum. Then， based on the criteria importance through intercriteria correlation（CRITIC）-entropy weight method， the optimal processing process of calcined Pyritum was optimized by orthogonal test. Powder XRD was used to analyze the phase of calcined Pyritum samples processed according to the best process， and the mean and median maps of calcined Pyritum were established by the superposition of geometric topological figures， and similarity evaluation and cluster analysis were carried out. ResultsThe results of single factor experiments showed that the physical phase of Pyritum changed from FeS2 to Fe7S8 during the process of temperature increase， the color gradually deepened from dark yellow， and the contents of heavy metals and harmful elements decreased. The optimized processing process of calcined Pyritum was as follows：calcination temperature at 750 ℃， calcination time of 2.5 h， paving thickness of 3 cm， particle size of 0.8-1.2 cm， vinegar quenching 1 time［Pyritum-vinegar（10∶3）］. After calcination， the internal structure of Pyritum was honeycomb-shaped， which was conducive to the dissolution of active ingredients. XRD fingerprints of 13 batches of calcined Pyritum characterized by 10 common peaks were established. The similarities of the relative peak intensities of the XRD fingerprints of the analyzed samples were>0.96， and it could effectively distinguish the raw products and unqualified products. ConclusionTemperature is the main factor affecting the quality of calcined Pyritum. After processing， the dissolution of the effective components in Pyritum increases， and the contents of heavy metals and harmful substances decrease， reflecting the function of processing to increase efficiency and reduce toxicity. The optimized processing process is stable and feasible， and the established XRD fingerprint can be used as one of the quality control standards of calcined Pyritum.
