目的 明确煅制温度对石决明Haliotidis Concha物相及成分组成的影响，优选石决明的炮制工艺，并对石决明药材及其饮片所含重金属元素含量进行对比及健康风险评估。方法 通过热重-差热分析（thermogravimetric-differential thermal analysis，TG-DTA）考察不同煅制温度下饮片的热效应发生过程，X射线衍射法（X-ray diffraction，XRD）考察主要物相转变，傅里叶变换红外光谱法（Fourier transform infrared spectroscopy，FTIR）考察成分组成变化，对影响石决明煅制工艺的关键因素“煅制温度”进行初筛。同时基于AHP-CRITIC混合加权法，结合正交试验，以CaCO₃含量、酥脆程度、色泽为评价指标，优选石决明的最佳炮制工艺参数；按最佳炮制工艺炮制饮片，采用电感耦合等离子体质谱法（inductively coupled plasma mass spectrometry，ICP-MS）对20批石决明药材及煅石决明饮片中Pb、Cd、As、Hg、Cu 5种重金属及有害元素进行测定分析；参考“中药中外源性有害残留物安全风险评估技术指导原则”与“中药有害残留物限量制定指导原则（通则9302），推算石决明中5种重金属及有害元素的最大限量理论值，同时计算其日暴露量和靶标危害系数（target hazard quotients，THQ）进行健康风险评估，为石决明的质量安全评价提供参考依据。结果 煅制温度初筛结果显示，煅制温度在400～600℃为宜，结合AHP-CRITIC混合加权法优选出石决明煅制工艺为取石决明药材，打碎至药材粒径＜1 cm，置马弗炉中，设置煅烧温度600℃，煅制90 min，即得。石决明煅制后有机质成分损失，CaCO₃含量相对增加，煅石决明饮片中As、Hg元素含量降低，Cu、Cd、Pb元素含量变化不大。健康风险评估结果显示，20批石决明药材及煅石决明饮片不会对人体健康产生明显的危害，且饮片中As、Hg元素含量显著低于药材（P＜0.05）。结论 结合药材炮制前后物相及成分变化，采用AHP-CRITIC混合加权法更加科学、全面地优选石决明煅制工艺，筛选结果科学可靠，为石决明药材及煅石决明饮片的质量管理和临床应用提供了新的科学依据。对石决明药材炮制前后重金属及有害元素进行健康风险评估，为石决明及其他贝壳类中药的临床安全用药提供参考。

Objective To investigate the effects of calcination temperature on the phase composition and chemical constituents of Shijueming (Haliotidis Concha, HC), optimize its processing methodology, and conduct comparative analysis and health risk assessment of heavy metal content in HC and calcined HC. Methods Thermal effects during processing at different calcination temperatures were examined via thermogravimetric-differential thermal analysis (TG-DTA). Primary phase transformations were analyzed using X-ray diffraction (XRD), while compositional changes were assessed by Fourier transform infrared spectroscopy (FTIR) to preliminarily screen the key factor “calcination temperature” affecting HC processing. Simultaneously, the optimal processing parameters for HC were determined using the AHP-CRITIC mixed entropy method combined with orthogonal experiments, with CaCO₃ content, crispness, and color as evaluation criteria. Calcined HC were processed according to the optimized method. Inductively coupled plasma mass spectrometry (ICP-MS) was employed to analyze 20 batches of HC and calcined HC for Pb, Cd, As, Hg, and Cu in 20 batches of HC and calcined calcined HC. Using HC powder as a reference, theoretical maximum limits for these five heavy metals and toxic elements were calculated. Daily exposure and target hazard quotient (THQ) were further assessed to evaluate health risks, providing a reference for quality and safety evaluation of HC. Results Preliminary screening of calcination temperatures indicated an optimal range of 400—600 ℃. Using the AHP-CRITIC mixed entropy method, the optimized calcination process for HC was determined as follows: Crush HC to a particle size < 1 cm, place in a muffle furnace, set the temperature to 600 ℃, and calcine for 90 min. After calcination, the organic matter content of HC decreased while calcium carbonate content increased. The calcined HC showed reduced levels of As and Hg, with minimal changes in Cu, Cd and Pb. Health risk assessment indicated that all 20 batches of HC and calcined HC posed no significant health hazards to humans. Notably, the As and Hg levels in the slices were significantly lower than those in the raw material (P < 0.05). Conclusion By integrating phase and compositional changes before and after processing, this study employed the AHP-CRITIC mixed entropy method to scientifically and comprehensively optimize the calcination process for HC. The screening results are scientifically reliable, providing new scientific evidence for quality management and clinical application of HC and calcined HC. Conducting health risk assessments of heavy metals and harmful elements in HC before and after processing provides reference for the safe clinical use of HC and other shell-derived Chinese medicinal materials.

R283.6

国家中医药管理局应用基础研究课题（gzyjc20210901）