1.Phlorizin Ameliorates Glucose and Lipid Metabolism Disorders in T2DM Rats by Modulating IRS-1/PI3K/Akt Signaling Pathway
Nuer AILI ; Qingyu CAO ; Huan LIU ; Junwei HE ; Weihong ZHONG ; Lan CAO
Chinese Journal of Experimental Traditional Medical Formulae 2026;32(3):139-148
ObjectiveTo observe the pharmacodynamic efficacy of phlorizin in improving hepatic glycolipid metabolism disorders in type 2 diabetic mellitus (T2DM) rats and to explore its mechanism of action based on the insulin receptor substrate-1 (IRS-1)/phosphatidylinositol 3-kinase (PI3K)/protein kinase B (Akt) signaling pathway. MethodsA high-fat diet and streptozotocin (STZ) were used to establish T2DM rat models. The rats were randomly assigned into six groups: the blank control group, model group, metformin group (300 mg·kg-1), and phlorizin high-dose (100 mg·kg-1) and low-dose groups (25 mg·kg-1). The rats were given intragastric administration for 6 weeks. The changes in body weight and fasting blood glucose (FBG) were observed, and the oral glucose tolerance test (OGTT) was carried out. The levels of total cholesterol (TC), triglyceride (TG), low-density lipoprotein cholesterol (LDL-C), high-density lipoprotein cholesterol (HDL-C), glycated serum protein (GSP), aspartate aminotransferase (AST), and alanine aminotransferase (ALT) in serum were detected by an automatic biochemical analyzer. The levels of fasting insulin (FINS), interleukin (IL)-1β, IL-6, and tumour necrosis factor (TNF)-α were detected by enzyme-linked immunosorbent assay (ELISA). The levels of superoxide dismutase (SOD) and malondialdehyde (MDA) were detected by the biochemical assays. The pancreas index, liver index, and insulin resistance index were calculated. Hematoxylin-eosin (HE) staining was used to evaluate the pathological changes in liver and pancreatic tissues. The immunofluorescence method was used to detect the changes in insulin and glucagon in pancreatic tissue. Western blot was used to detect the expression of related proteins in the IRS-1/PI3K/Akt pathway of liver tissue and its downstream glycogen synthase kinase-3β (GSK-3β) and forkhead box transcription factor O1 (FoxO1) proteins. ResultsCompared with the blank control group, the body weight of rats in the model group continued to decrease, while the FBG level increased significantly. The area under the OGTT blood glucose curve (AUC), GSP, TC, TG, LDL-C, IL-1β, IL-6, TNF-α, MDA, pancreatic index and liver index increased significantly, while the levels of HDL-C, SOD, and FINS decreased significantly (P0.05, P0.01). Histological results showed that the pancreatic islets of rats in the model group exhibited atrophy and severe structural abnormalities. The insulin-positive β-cells decreased significantly (P0.01), while the glucagon-positive α-cells increased significantly (P0.01). Inflammatory cell infiltration and partial necrosis were observed in the liver tissues of the model group rats. The expressions of p-IRS-1/IRS-1, p-GSK-3β/GSK-3β, and p-FoxO1/FoxO1 proteins in the liver of the model group increased significantly (P0.01), while the expressions of p-PI3K/PI3K and p-Akt/Akt proteins decreased significantly (P0.01). Compared with the model group, the diabetic symptoms of rats in all administration groups were improved. The changes in body weight and FBG were close to those of the blank control group. The levels of OGTT-AUC, GSP, TC, TG, LDL-C, MDA, IL-1β, IL-6, TNF-α and the pancreatic index, liver index were obviously reduced (P0.05, P0.01), while the levels of HDL-C, SOD, and FINS obviously increased (P0.05, P0.01). The pathological changes of the pancreas and liver in rats in all treatment groups were effectively improved. The insulin-positive β-cells in the pancreas increased significantly (P0.01), while the glucagon-positive α-cells decreased significantly (P0.01). The protein expressions of p-IRS-1/IRS-1, p-GSK-3β/GSK-3β, and p-FoxO1/FoxO1 in the liver were significantly reduced (P0.01), while the protein expressions of p-PI3K/PI3K and p-Akt/Akt significantly increased (P0.01). ConclusionPhlorizin reversed the weight loss and abnormal increase of FBG in T2DM rats, improved blood lipid profiles, oxidative stress, and inflammatory levels, alleviated insulin resistance, and had certain protective effects on the liver and pancreas. The hypoglycemic mechanism may involve regulating the IRS-1/PI3K/Akt signaling pathway to inhibit the activities of GSK-3β and FoxO1, thereby promoting liver glycogen synthesis and suppressing hepatic gluconeogenesis, ultimately improving glycolipid metabolism disorders.
2.Phlorizin Ameliorates Glucose and Lipid Metabolism Disorders in T2DM Rats by Modulating IRS-1/PI3K/Akt Signaling Pathway
Nuer AILI ; Qingyu CAO ; Huan LIU ; Junwei HE ; Weihong ZHONG ; Lan CAO
Chinese Journal of Experimental Traditional Medical Formulae 2026;32(3):139-148
ObjectiveTo observe the pharmacodynamic efficacy of phlorizin in improving hepatic glycolipid metabolism disorders in type 2 diabetic mellitus (T2DM) rats and to explore its mechanism of action based on the insulin receptor substrate-1 (IRS-1)/phosphatidylinositol 3-kinase (PI3K)/protein kinase B (Akt) signaling pathway. MethodsA high-fat diet and streptozotocin (STZ) were used to establish T2DM rat models. The rats were randomly assigned into six groups: the blank control group, model group, metformin group (300 mg·kg-1), and phlorizin high-dose (100 mg·kg-1) and low-dose groups (25 mg·kg-1). The rats were given intragastric administration for 6 weeks. The changes in body weight and fasting blood glucose (FBG) were observed, and the oral glucose tolerance test (OGTT) was carried out. The levels of total cholesterol (TC), triglyceride (TG), low-density lipoprotein cholesterol (LDL-C), high-density lipoprotein cholesterol (HDL-C), glycated serum protein (GSP), aspartate aminotransferase (AST), and alanine aminotransferase (ALT) in serum were detected by an automatic biochemical analyzer. The levels of fasting insulin (FINS), interleukin (IL)-1β, IL-6, and tumour necrosis factor (TNF)-α were detected by enzyme-linked immunosorbent assay (ELISA). The levels of superoxide dismutase (SOD) and malondialdehyde (MDA) were detected by the biochemical assays. The pancreas index, liver index, and insulin resistance index were calculated. Hematoxylin-eosin (HE) staining was used to evaluate the pathological changes in liver and pancreatic tissues. The immunofluorescence method was used to detect the changes in insulin and glucagon in pancreatic tissue. Western blot was used to detect the expression of related proteins in the IRS-1/PI3K/Akt pathway of liver tissue and its downstream glycogen synthase kinase-3β (GSK-3β) and forkhead box transcription factor O1 (FoxO1) proteins. ResultsCompared with the blank control group, the body weight of rats in the model group continued to decrease, while the FBG level increased significantly. The area under the OGTT blood glucose curve (AUC), GSP, TC, TG, LDL-C, IL-1β, IL-6, TNF-α, MDA, pancreatic index and liver index increased significantly, while the levels of HDL-C, SOD, and FINS decreased significantly (P0.05, P0.01). Histological results showed that the pancreatic islets of rats in the model group exhibited atrophy and severe structural abnormalities. The insulin-positive β-cells decreased significantly (P0.01), while the glucagon-positive α-cells increased significantly (P0.01). Inflammatory cell infiltration and partial necrosis were observed in the liver tissues of the model group rats. The expressions of p-IRS-1/IRS-1, p-GSK-3β/GSK-3β, and p-FoxO1/FoxO1 proteins in the liver of the model group increased significantly (P0.01), while the expressions of p-PI3K/PI3K and p-Akt/Akt proteins decreased significantly (P0.01). Compared with the model group, the diabetic symptoms of rats in all administration groups were improved. The changes in body weight and FBG were close to those of the blank control group. The levels of OGTT-AUC, GSP, TC, TG, LDL-C, MDA, IL-1β, IL-6, TNF-α and the pancreatic index, liver index were obviously reduced (P0.05, P0.01), while the levels of HDL-C, SOD, and FINS obviously increased (P0.05, P0.01). The pathological changes of the pancreas and liver in rats in all treatment groups were effectively improved. The insulin-positive β-cells in the pancreas increased significantly (P0.01), while the glucagon-positive α-cells decreased significantly (P0.01). The protein expressions of p-IRS-1/IRS-1, p-GSK-3β/GSK-3β, and p-FoxO1/FoxO1 in the liver were significantly reduced (P0.01), while the protein expressions of p-PI3K/PI3K and p-Akt/Akt significantly increased (P0.01). ConclusionPhlorizin reversed the weight loss and abnormal increase of FBG in T2DM rats, improved blood lipid profiles, oxidative stress, and inflammatory levels, alleviated insulin resistance, and had certain protective effects on the liver and pancreas. The hypoglycemic mechanism may involve regulating the IRS-1/PI3K/Akt signaling pathway to inhibit the activities of GSK-3β and FoxO1, thereby promoting liver glycogen synthesis and suppressing hepatic gluconeogenesis, ultimately improving glycolipid metabolism disorders.
3.Correlation of serum leucine-rich α-2 glycoprotein 1 and fibroblast growth factor 21 levels with neovascular glaucoma
Zhong LUO ; He ZHOU ; Yi HUANG ; Wanjiang DONG
International Eye Science 2025;25(1):118-121
AIM: To investigate the correlation of serum leucine-rich α-2 glycoprotein 1(LRG1)and fibroblast growth factor 21(FGF-21)levels with neovascular glaucoma(NVG).METHODS: A total of 110 cases(110 eyes)with NVG admitted to the ophthalmology department from September 2020 to September 2022 were selected as NVG group, with 23 cases of grade II, 44 cases of grade III, and 43 cases of grade IV, while 90 sex and age matched cataract patients(90 eyes)were selected as control group. The levels of LRG1, FGF-21, vascular endothelial growth factor(VEGF), pigment epithelium-derived factor(PEDF), and tumor necrosis factor-α(TNF-α)in serum were detected by ELISA; Pearson correlation analysis was used to analyze the correlation of serum LRG1 and FGF-21 levels with Teich grade, VEGF, PEDF and TNF-α levels.RESULTS: The levels of serum LRG1, FGF-21, VEGF, PEDF and TNF-α in the NVG group were significantly higher than those in the control group(all P<0.01). With the increase of Teich grading, the levels of serum LRG1, FGF-21, VEGF, PEDF and TNF-α in NVG patients significantly increased in turn(all P<0.05). Correlation analysis showed that the levels of LRG1 and FGF-21 in serum of NVG patients were positively correlated with the levels of VEGF, PEDF and TNF-α(all P<0.05).CONCLUSION: The levels of LRG1 and FGF-21 in serum of patients with NVG are obviously increased, which are positively correlated with the levels of VEGF, PEDF and TNF-α, both of which may be related to the development of NVG.
4.Working practices in eliminating the public health crisis caused by viral hepatitis in Hainan Province of China
Weihua LI ; Changfu XIONG ; Taifan CHEN ; Bin HE ; Dapeng YIN ; Xuexia ZENG ; Feng LIN ; Biyu CHEN ; Xiaomei ZENG ; Biao WU ; Juan JIANG ; Lu ZHONG ; Yuhui ZHANG
Journal of Clinical Hepatology 2025;41(2):228-233
In 2022, Hainan provincial government launched the project for the prevention and control of viral hepatitis with the goals of a hepatitis B screening rate of 90%, a diagnostic rate of 90%, and a treatment rate of 80% among people aged 18 years and above by the year 2025, and the main intervention measures include population-based prevention, case screening, antiviral therapy, and health management. As of December 31, 2024, a total of 6.875 million individuals in the general population had been screened for hepatitis B, with a screening rate of 95.6%. A total of 184 710 individuals with positive HBsAg were identified, among whom 156 772 were diagnosed through serological reexamination, resulting in a diagnostic rate of 84.9%. A total of 50 742 patients with chronic hepatitis B were identified, among whom 42 921 had hepatitis B-specific health records established for health management, with a file establishment rate of 84.6%. A total of 31 553 individuals received antiviral therapy, with a treatment rate of 62.2%. A total of 2.503 million individuals at a high risk of hepatitis C were screened, among whom 4 870 tested positive for HCV antibody and 3 858 underwent HCV RNA testing, resulting in a diagnostic rate of 79.2%, and 1 824 individuals with positive HCV RNA were identified, among whom 1 194 received antiviral therapy, with a treatment rate of 65.5%. In addition, 159 301 individuals with negative HBsAg and anti-HBs and an age of 20 — 40 years were inoculated with hepatitis B vaccine free of charge. Through the implementation of the project for the prevention and control of viral hepatitis, a large number of hepatitis patients have been identified, treated, and managed in the province within a short period of time, which significantly accelerates the efforts to eliminate the crisis of viral hepatitis.
5.A Fitting Method for Photoacoustic Pump-probe Imaging Based on Phase Correction
Zhuo-Jun XIE ; Hong-Wen ZHONG ; Run-Xiang LIU ; Bo WANG ; Ping XUE ; Bin HE
Progress in Biochemistry and Biophysics 2025;52(2):525-532
ObjectivePhotoacoustic pump-probe imaging can effectively eliminate the interference of blood background signal in traditional photoacoustic imaging, and realize the imaging of weak phosphorescence molecules and their triplet lifetimes in deep tissues. However, background differential noise in photoacoustic pump-probe imaging often leads to large fitting results of phosphorescent molecule concentration and triplet lifetime. Therefore, this paper proposes a novel triplet lifetime fitting method for photoacoustic pump-probe imaging. By extracting the phase of the triplet differential signal and the background noise, the fitting bias caused by the background noise can be effectively corrected. MethodsThe advantages and feasibility of the proposed algorithm are verified by numerical simulation, phantom and in vivo experiments, respectively. ResultsIn the numerical simulation, under the condition of noise intensity being 10% of the signal amplitude, the new method can optimize the fitting deviation from 48.5% to about 5%, and has a higher exclusion coefficient (0.88>0.79), which greatly improves the fitting accuracy. The high specificity imaging ability of photoacoustic pump imaging for phosphorescent molecules has been demonstrated by phantom experiments. In vivo experiments have verified the feasibility of the new fitting method proposed in this paper for fitting phosphoometric lifetime to monitor oxygen partial pressure content during photodynamic therapy of tumors in nude mice. ConclusionThis work will play an important role in promoting the application of photoacoustic pump-probe imaging in biomedicine.
6.Role of neutrophil in fungal keratitis
Junming YANG ; Yanting LUO ; Hong HE ; Xingwu ZHONG
International Eye Science 2025;25(2):230-234
Fungal keratitis represents a significant cause of blindness, with current therapeutic approaches yielding limited success. The disease's onset and progression are primarily driven by fungal virulence factors and the host's immune response. The innate immune system is the first to respond, with neutrophils playing a pivotal role in the antifungal defense. Although neutrophils are critical for pathogen clearance, their excessive or abnormal activation can lead to tissue damage, exacerbating the disease. Thus, elucidating the mechanisms underlying neutrophil activity in fungal keratitis is crucial for refining treatment strategies. This article aims to systematically review the principal antimicrobial mechanisms employed by neutrophils, including phagocytosis, degranulation, and the formation of neutrophil extracellular traps(NETs). Furthermore, it explores the crosstalk between neutrophils and macrophages, alongside their collective impact and underlying mechanisms in the context of fungal keratitis. Exploration of the mechanisms of fungal keratitis facilitates precise intervention and enhances the efficacy of treatment.
7.Optimization of Processing Technology of Calcined Pyritum Based on QbD Concept and Its XRD Fingerprint Analysis
Xin CHEN ; Jingwei ZHOU ; Haiying GOU ; Lei ZHONG ; Tianxing HE ; Wenbo FEI ; Jialiang ZOU ; Yue YANG ; Dewen ZENG ; Lin CHEN ; Hongping CHEN ; Shilin CHEN ; Yuan HU ; Youping LIU
Chinese Journal of Experimental Traditional Medical Formulae 2025;31(13):197-205
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.
8.Assessing distribution characteristics and clinical significance of vertebral fractures in patients with osteoporosis based on whole spine MRI
Jiajun ZHOU ; Fei MA ; Yebo LENG ; Shicai XU ; Baoqiang HE ; Yang LI ; Yehui LIAO ; Qiang TANG ; Chao TANG ; Qing WANG ; Dejun ZHONG
Chinese Journal of Tissue Engineering Research 2025;29(9):1883-1889
BACKGROUND:Osteoporotic vertebral fractures are the most common complication in patients with osteoporosis.As a new imaging technique,spine magnetic resonance imaging(MRI)is much more sensitive than X-ray film in the diagnosis of osteoporotic vertebral fractures.However,total spine MRI is costly and takes a long time to scan.Therefore,there is no consensus on whether all patients with osteoporotic vertebral fractures need to undergo total spine MRI scan and which patients need to undergo total spine MRI. OBJECTIVE:To analyze the distribution characteristics of vertebral fractures and explore their clinical significance by observing the whole spine MRI data of osteoporotic vertebral fractures patients. METHODS:Data of cases and MRI images of all patients diagnosed with fresh osteoporotic vertebral fractures who visited the Department of Orthopedics,Affiliated Hospital of Southwest Medical University from August 2018 to September 2022 were retrospectively analyzed.903 patients were included in the study based on inclusion and exclusion criteria.General information(age,gender,and body mass index),medical history characteristics(duration of illness,history of trauma surgery,percussion pain area,and pain score)were collected.The characteristics of vertebral fractures were analyzed through whole spine magnetic resonance imaging.Firstly,based on the number of vertebral fractures in patients,they were divided into the single vertebral fracture group(484 cases)and the multi-vertebral fracture group(419 cases),and the differences were analyzed between the two groups.Then,based on whether the farthest interval between the fractured vertebrae was greater than or equal to 5,the multi vertebral fracture group was further divided into two subgroups.Among them,Group A(the farthest interval between the fractured vertebrae was less than 5)contained 306 cases;Group B(with the farthest interval between fractured vertebral bodies greater than 5)included 113 cases.The differences were analyzed between two subgroups. RESULTS AND CONCLUSION:(1)Among 903 patients,419 patients(46.4%)had more than two fractured vertebrae.There were 654 patients(72.4%)with thoracolumbar fractures,and 54 patients(6%)with fractures in the thoracic plus lumbar region and the entire thoracic to lumbar region.In group B,96.5%of patients had multiregional percussion pain.(2)Compared with the patients in the single vertebral fracture group and the multi-vertebral fracture group,there were significant differences in bone mineral density,whether the medical history was greater than or equal to 1 month,the history of low energy injury,and the distribution and number of axial percussion pain areas in the spine during physical examination between the two groups(P<0.05).Age,gender,body mass index,whether there was underlying disease,pain visual analog scale score,whether there was a history of elderly thoracolumbar fracture,and whether there was a history of thoracolumbar surgery,and the number of fractured vertebrae had no statistical significance(P>0.05).(3)There were statistically significant differences between the Groups A and B in bone mineral density,the distribution and quantity of percussion pain area,and the history of low energy injury(P<0.05).There were no significant differences in age,gender,history of old fractures,visual analog scale score,body mass index,whether the medical history was longer than or equal to 1 month,history of underlying diseases,and history of thoracolumbar surgery between the two groups(P>0.05).(4)Patients with multiple low-energy trauma history,history of more than 1 month,multiple percussion pain,and the lower bone mineral density should be alert to the occurrence of multiple vertebral fracture and jump fracture.We recommend the whole spinal MRI for these patients.
9.Effect of Shenmai injection on the preservation quality of suspended red blood cells prepared from high hemoglobin population in Xizang plateau
Rui ZHONG ; Zeng HE ; Hong WANG ; Wanjing LI ; Jiaxin LIU ; Ye CAO
Chinese Journal of Blood Transfusion 2025;38(3):327-332
[Objective] To investigate the effect of Shenmai injection on the preservation quality of suspended red blood cells of high hemoglobin population in Xizang plateau. [Methods] Whole blood (400 mL, n=8) collected by the Xizang Autonomous Region Blood Center was centrifuged at 3 000 g for 10 minutes to remove most of the plasma, followed by the addition of 100 mL of MAP preservation solution to obtain plateau suspended red blood cells, which were then divided into three equal portions. One portion was the control group, and another part had 15 mL of MAP preservation solution added, which was the dosage group. The third portion involved diluting Shenmai injection with MAP, followed by addition of 15 mL of MAP preservation solution containing Shenmai to the red blood cells, resulting in a final concentration of Shenmai injection of 1%, which was the Shenmai group. Blood routine, pH value, electrolytes, glucose, lactate, free Hb, adenosine triphosphate (ATP), P50, phosphatidylserine (PS) and other indicators were detected at day 1, 21 and 35, respectively. [Results] The Hb concentration and Hct of the dosage group and the Shenmai group were significantly lower than those of the control group, with values of (179.3±17.8) vs (181.0±17.1) vs (199.1±19.5) g/L for Hb concentration and (53.2±2.6)% vs (53.3±2.5)% vs (58.4±3.1)% for Hct. The three groups maintained this pattern until the end of storage. In the middle and late stages of preservation, the glucose and Na+ contents in the dosage group and the Shenmai group were higher than those in the control group, while the lactate and K+ contents were lower than those in the control group. At the end of storage, the glucose and Na+ content of the Shenmai group was higher than that of the dosage group, while the lactate and K+ content were lower than that of the dosage group. From day 1 to day 35 of storage, the hemolysis rate of the Shenmai group was significantly lower than that of the control group and the dosage group. On day 21 and 35 of storage, the PS expression rate in the Shenmai group was significantly lower than that in the control group and the dosage group, which were (6.52±0.40)% vs (7.24±0.91)% vs (8.27±0.93)% and (7.29±0.53)% vs (9.37±0.82)% vs (8.39±0.76)%, respectively. [Conclusion] The hemolysis rate and PS of suspended red blood cells of Xizang high altitude prepared by adding Shenmai injection were significantly lower than those in the control group and the dosage group, which was conducive to reducing hemolysis and slowing down the aging of red blood cells, and had a certain improvement on the preservation quality of suspended red blood cells in Xizang plateau people.
10.Optimization of Processing Technology of Calcined Pyritum Based on QbD Concept and Its XRD Fingerprint Analysis
Xin CHEN ; Jingwei ZHOU ; Haiying GOU ; Lei ZHONG ; Tianxing HE ; Wenbo FEI ; Jialiang ZOU ; Yue YANG ; Dewen ZENG ; Lin CHEN ; Hongping CHEN ; Shilin CHEN ; Yuan HU ; Youping LIU
Chinese Journal of Experimental Traditional Medical Formulae 2025;31(13):197-205
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.

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