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基于多技术联合表征的市售煅磁石饮片质量评价

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中草药 | 药剂与工艺 2026,57(8): 3072-3084

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中草药 |药剂与工艺 2026 , 57 (8) : 3072 -3084

基于多技术联合表征的市售煅磁石饮片质量评价

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曾德雯¹, 周靖惟¹, 杨玥¹, 钟磊², 陈欣¹, 费文波², 赵亮¹, 王福¹, 陈鸿平¹, 陈林¹, 陈士林³, 胡媛¹, 刘友平¹

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通讯作者:

胡媛

作者简介:

曾德雯: 曾德雯(2000-),女,硕士研究生,从事中药药效物质与质量评价研究。E-mail:2770587942@qq.com

Research on quality evaluation of commercially available calcined Magnetitum decoction slices based on multi-technology integrated characterization

ZENG Dewen, ZHOU Jingwei, YANG Yue, ZHONG Lei, CHEN Xin, FEI Wenbo, ZHAO Liang, WANG Fu, CHEN Hongping, CHEN Lin, CHEN Shilin, HU Yuan, LIU Youping

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doi: 10.7501/j.issn.0253-2670.2026.08.020

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目的采用多技术联合表征市售煅磁石饮片，探索煅磁石饮片质量评价方法。方法收集11批市售煅磁石饮片，根据《中国药典》2025年版一部进行质量检查；采用热分析（thermal analysis，TA）、X射线衍射（X-ray diffraction，XRD）、X射线荧光（X-ray fluorescence，XRF）、傅里叶变换红外光谱（fourier transform infrared spectroscopy，FTIR）表征样品的热稳定性、物相组成、元素组成、红外结构；采用电感耦合等离子体（inductively coupled plasma mass spectrometry，ICP-MS）测定样品的重金属及有害元素含量，计算最大残留量限量理论值（L）和靶标危害系数（target hazard quotient，THQ），评估其健康风险。结果 11批市售煅磁石饮片含量测定结果合格，但有4批饮片性状存在颜色偏红的质量问题，不符合《中国药典》2025年版一部煅磁石颜色的规定。TA结果显示，11批市售煅磁石饮片的热稳定性差异较大，其中有5批饮片缓慢失重、有4批饮片在420～580 ℃出现失重台阶、有2批饮片先增重后又在420～580℃出现失重台阶。XRD结果显示，市售煅磁石饮片主要有Fe₃O₄、SiO₂及Fe₂O₃ 3种物相，其中Fe₂O₃的相对衍射强度差异大。XRF结果显示，市售煅磁石饮片主要由Fe、Si、Al、Mg、P、K、Ca组成，Fe、Si的相对含量达90%。FTIR结果显示，市售煅磁石饮片在1 250～1 100、800～600、600～300 cm⁻¹ 3个波段分别出现Si-O非对称轴伸缩振动、Si-O-Si对称伸缩振动、Si-O弯曲振动的吸收峰，在540～570 cm⁻¹出现Fe-O伸缩振动吸收峰。ICP-MS结果显示，11批市售煅磁石饮片中，有3批饮片的Hg含量大于L，THQ＞1；有1批饮片的Pb含量大于L，THQ＞1。结论基于《中国药典》2025年版和多种技术结合对煅磁石饮片进行质量评价，以期为煅磁石饮片的质量控制水平提升、质量提高提供参考。

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

Abstract

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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 of 420—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.

Key words

calcined Magnetitum / X-ray diffraction / thermal analysis technology / Fourier transform infrared spectroscopy / inductively coupled plasma mass spectrometry / quality evaluation / health risk assessment

引用本文

曾德雯, 周靖惟, 杨玥, 钟磊, 陈欣, 费文波, 赵亮, 王福, 陈鸿平, 陈林, 陈士林, 胡媛, 刘友平. 基于多技术联合表征的市售煅磁石饮片质量评价. 中草药, 2026 , 57 (8) : 3072 -3084 . DOI: 10.7501/j.issn.0253-2670.2026.08.020

ZENG Dewen, ZHOU Jingwei, YANG Yue, ZHONG Lei, CHEN Xin, FEI Wenbo, ZHAO Liang, WANG Fu, CHEN Hongping, CHEN Lin, CHEN Shilin, HU Yuan, LIU Youping. Research on quality evaluation of commercially available calcined Magnetitum decoction slices based on multi-technology integrated characterization[J]. Chinese Traditional and Herbal Drugs, 2026 , 57 (8) : 3072 -3084 . DOI: 10.7501/j.issn.0253-2670.2026.08.020

基金

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2018年中央部门预算全国中药资源普查项目 (GZY-KJS-2018-004); 第四次全国中药资源普查项目 (GZY-KJS-2019-001)

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2026年第57卷第8期

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doi: 10.7501/j.issn.0253-2670.2026.08.020

接收时间：2025-11-04
首发时间：2026-09-09

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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