目的 通过分析炒九香虫Aspongopus饮片制备为配方颗粒过程中的指标性成分与挥发性气味物质变化，探究其量值传递与气味变化规律。方法 采用Cosmosil 5C₁₈-MS-II色谱柱（250 mm×4.6 mm，5 μm），乙腈-0.1%甲酸水溶液为流动相，梯度洗脱，建立HPLC分析方法，探讨炒九香虫饮片、标准汤剂与配方颗粒间的指标成分转移率。采用顶空固相微萃取（headspace solid-phase microextraction，HS-SPME）-气相色谱-质谱联用（gas chromatography-mass spectrometry，GC-MS）技术对炒九香虫饮片、标准汤剂、配方颗粒的挥发性成分进行鉴定和比较。通过计算气味活度值（odor activity value，OAV）评估各成分的气味贡献度，以确定关键气味成分；结合NIST05a数据库和多元统计分析，分析挥发性成分及气味变化规律。结果 炒九香虫饮片到标准汤剂工艺过程中，腺嘌呤的转移率为76.03%～96.01%，犬尿喹啉酸的转移率为62.75%～95.06%；炒九香虫标准汤剂到配方颗粒工艺过程中，腺嘌呤的转移率为88.90%～94.95%，犬尿喹啉酸的转移率为69.48%～80.79%。炒九香虫饮片、标准汤剂与配方颗粒分别检测出79、69及65种挥发性成分，其中异戊酸、己酸、丁酸既是关键气味成分也是差异标志物。由炒九香虫饮片到标准汤剂的浸泡、煎煮工艺使酸类挥发性难闻成分含量减少79.32%，经进一步制粒后，配方颗粒相比饮片的酸类挥发性难闻成分含量减少了91.03%，并且新增加了具有焦香气味的甲基麦芽酚。结论 炒九香虫饮片、标准汤剂、配方颗粒的腺嘌呤和犬尿喹啉酸传递稳定，所建立的HPLC分析方法为炒九香虫配方颗粒质量控制提供参考；炒九香虫配方颗粒的气味相比饮片和标准汤剂得到改善。

Objective In this study, the changes of index components and volatile substances in the preparation of stir-baked Jiuxiangchong (Aspongopus) decoction pieces into formula granules were analyzed, and the value transmission and volatile odor changes were explored. Methods Cosmosil 5C₁₈-MS-II column (250 mm×4.6 mm, 5 μm) with acetonitrile-0.1% formic acid in water as mobile phase was used for gradient elution. An HPLC analysis method was established to explore the transfer rate of index components between decoction pieces, standard decoction and formula granules. Headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) was used to identify and compare the volatile components of stir-baked Aspongopus decoction pieces, standard decoction and formula granules. The odor contribution of each component was evaluated by calculating the odor activity value (OAV) to identify the key odor components. Combined with the NIST05a database and multivariate statistical analysis, the volatile components and odor changes were analyzed. Results The transfer rate of stir-baked Aspongopus decoction pieces to standard decoction adenine was 76.03%—96.01%, and the transfer rate of kynurenic acid was 62.75%—95.06%. The transfer rate from the standard decoction of stir-baked Aspongopus to the formula granules adenine was 88.90%—94.95%, and the transfer rate of kynurenic acid was 69.48%—80.79%. A total of 79, 69 and 65 volatile components were detected in the stir-baked Aspongopus decoction pieces, standard decoction and formula granules, respectively, among which isovaleric acid, caproic acid and butyric acid were the key odor components and difference markers. The content of volatile and unpleasant smell components of acids was reduced by 79.32% by the soaking and decoction process from stir-baked Aspongopus decoction pieces to standard decoction, and after further granulation, the content of volatile and unpleasant components of acid volatile components of the formula granules was reduced by 91.03% compared with that of decoction pieces, and methyl maltol with burnt smell was newly added. Conclusion The transmission of adenine and kynurenic acid in stir-baked Aspongopus decoction pieces, standard decoction and formula granules was stable, and the established HPLC analysis method provided a reference for the quality control of stir-baked Aspongopus formula granules. The smell of stir-baked Aspongopus formula granules was improved compared to decoction pieces and standard decoctions.

R283.6

国家自然科学基金项目（82173991）