中草药2026,Vol.57Issue(8):3072-3084,13.DOI:10.7501/j.issn.0253-2670.2026.08.020
基于多技术联合表征的市售煅磁石饮片质量评价
Research on quality evaluation of commercially available calcined Magnetitum decoction slices based on multi-technology integrated characterization
摘要
Abstract
Objective To apply multiple techniques for the combined characterization of commercially available calcined Magnetitum decoction slices and to explore the quality evaluation methods for calcined Magnetitum decoction slices.Methods Eleven batches of commercially available calcined Magnetitum decoction slices were collected.Quality inspections were carried out in accordance with the 2025 edition of the Chinese Pharmacopoeia(volume Ⅰ).Thermal analysis(TA),X-ray diffraction(XRD),X-ray fluorescence(XRF),and Fourier transform infrared spectroscopy(FTIR)were utilized to characterize the thermal stability,phase composition,elemental composition,and infrared structure of the samples.Inductively coupled plasma mass spectrometry(ICP-MS)was used to determine the contents of heavy metals and harmful elements in the samples.The theoretical maximum residue limit value L and the target hazard quotient(THQ)were calculated to evaluate the health risks.Results The content determination results of 11 batches of commercially available calcined Magnetitum decoction slices were qualified,but the appearance of 4 batches of slices had a quality issue of being too red,which did not meet the requirements of the 2025 edition of the Chinese Pharmacopoeia(volume Ⅰ).TA results indicated significant differences in the thermal stability of the 11 batches of commercially available calcined Magnetitum decoction slices.Five batches showed a slow weight loss trend;four batches presented weight loss steps in the temperature range of420-580 °℃;two batches first showed weight gain and then weight loss steps in the 420-580 °℃ range.XRD results showed that the commercially available calcined Magnetitum decoction slices mainly consisted of three phases:Fe3O4,SiO2,and Fe2O3,with significant differences in the relative diffraction intensity of Fe2O3.XRF results demonstrated that the commercially available calcined Magnetitum decoction slices were mainly composed of elements such as Fe,Si,Al,Mg,P,K,and Ca,and the relative contents of Fe and Si reached 90%.FTIR results showed that the commercially available calcined Magnetitum decoction slices exhibited characteristic absorption peaks of Si-O asymmetric stretching vibration,Si-O-Si symmetric stretching vibration,and Si-O bending vibration in the three wavelength bands of 1 250-1 100,800-600,and 600-300 cm-1,respectively,and an absorption peak of Fe-O stretching vibration appeared in the 540-570 cm-1 band.ICP-MS results indicated that among 11 batches of commercially available calcined Magnetitum decoction slices,three batches exhibited mercury(Hg)content exceeding the limit L with a THQ greater than 1;One batch showed lead(Pb)content exceeding the limit L with THQ>1.Conclusion The quality of calcined Magnetitum decoction slices was evaluated based on the 2025 edition of the Chinese Pharmacopoeia and multiple techniques,with the aim of providing a reference for improving the quality control of calcined Magnetitum decoction slices.关键词
煅磁石/X射线衍射/热分析技术/傅里叶变换红外光谱/电感耦合等离子体质谱/质量评价/健康风险评估Key words
calcined Magnetitum/X-ray diffraction/thermal analysis technology/Fourier transform infrared spectroscopy/inductively coupled plasma mass spectrometry/quality evaluation/health risk assessment分类
医药卫生引用本文复制引用
曾德雯,陈林,陈士林,胡媛,刘友平,周靖惟,杨玥,钟磊,陈欣,费文波,赵亮,王福,陈鸿平..基于多技术联合表征的市售煅磁石饮片质量评价[J].中草药,2026,57(8):3072-3084,13.基金项目
2018年中央部门预算全国中药资源普查项目(GZY-KJS-2018-004) (GZY-KJS-2018-004)
第四次全国中药资源普查项目(GZY-KJS-2019-001) (GZY-KJS-2019-001)