广藿香药材及饮片质量标准提升研究

目的 修订和完善广藿香药材和饮片质量标准，为合理控制广藿香药材和饮片质量提供科学依据。方法 分别收集23批广藿香药材和32批饮片代表性样品，参照《中华人民共和国药典》2020年版广藿香项下标准修订叶片粉末的显微鉴别方法；简化薄层色谱鉴别前处理方法，建立以广藿香对照药材和百秋李醇对照品为对照的薄层色谱鉴别方法；改进含量测定项下供试品制备方法，修订药材指标性成分限度；新增广藿香饮片标准检查、浸出物和含量测定项。结果 建议显微鉴别中腺鳞头部细胞描述为“细胞壁多破裂而呈裂隙状”；薄层色谱方法中用石油醚超声提取、乙酸乙酯复溶代替原标准中提取挥发油的前处理方式，以5%茴香醛浓硫酸溶液为显色剂，所有样品与广藿香对照药材和百秋李醇对照品在同一位置显相同颜色的斑点，改进后方法前处理简单、展开效果好、斑点清晰；建议适当提高药材醇溶性浸出物限度，用乙醇作溶剂时不低于4.0%；采用无水乙醇替换毒性较大的三氯甲烷作为含量测定提取溶剂，方法学考察符合要求，23批广藿香药材百秋李醇质量分数和平均值分别为0.34%~0.92%、0.58%，建议药材标准中提高百秋李醇质量分数限度为0.22%；新增饮片检查项目，其中水分不得过14.0%，总灰分不得过11.0%，酸不溶性灰分不得过4.0%；新增饮片浸出物项目，限度同药材标准；新增饮片含量测定项，32批饮片中百秋李醇质量分数和平均值分别为0.12%~0.46%、0.29%，建议饮片中百秋李醇质量分数不低于0.20%。结论 所建立的方法操作简便可行、准确可靠、重复性好，新增项目和制订的标准限度合理，可用于广藿香药材和饮片的质量控制。

Study on Quality Standards Improvement of Pogostemonis Herba Medicinal Materials and Decoction Pieces

Objective To revise and improve quality standards of Pogostemonis Herba medicinal materials and decoction pieces, further provide scientific basis for rational control of the quality.Methods A total of 23 batches of Pogostemonis Herba and 32 batches of representative decoction pieces were collected. The leaf powder was microscopically identified with reference to the Chinese Pharmacopoeia (2020 edition). The existing pre-treatment method for thin-layer chromatographic (TLC) identification was simplified to establish a new TLC identification using Pogostemonis Herba reference material and patchouli alcohol reference substance as the controls. Moreover, the sample preparation method for content determination was improved, and the limits of index components in medicinal materials were revised. The inspection on Pogostemonis Herba decoction pieces standard, leachate and content determination were added.Results It was suggested that the microscopic identification of glandular squamous head cells should be described as having a fissured cell wall with multiple ruptures. Ultrasonic extraction with petroleum ether and re-dissolution with ethyl acetate were adopted instead of original extraction of volatile oil as a pretreatment in TLC. With 5% anisaldehyde concentrated sulfuric acid solution was used as the chromogenic agent, all samples, patchouli reference medicinal material and patchouli alcohol reference substance all showed the spots in the same color at the same position. The pretreatment was simplified after improvements, the development efficacy was good, and the spots were distinct. It was suggested that the limit of alcohol-soluble extracts of medicinal materials should be appropriately increased to no less than 4.0% when ethanol was used as the solvent. Anhydrous ethanol was used to replace the original toxic chloroform as the extraction solvent for content determination. The methodological investigation met with the requirements. The mass fractions and average value of patchouli alcohol in the 23 batches of Pogostemonis Herba medicinal materials were 0.34%-0.92% and 0.58%, respectively. It was recommended that the limit of patchouli alcohol content in the medicinal materials should be increased to 0.22%. Moreover, new items for inspection were added for decoction pieces, including moisture content no higher than 14.0%, total ash content no higher than 11.0%, and acid insoluble ash content no higher than 4.0%. The item for leachate from decoction pieces was added and the limit was the same to that of the medicinal material standards. The item for content determination of decoction pieces was added, the mass fraction and average of patchouli alcohol in the 32 batches of decoction pieces were 0.12%-0.46% and 0.29%, respectively, and it was recommended that the content of patchouli alcohol should be no less than 0.20%.Conclusion The method is simple, feasible, accurate, reliable, and highly reproducible. The new items and the standard limits are reasonable. They can be used for the quality control of Pogostemonis Herba medicinal materials and decoction pieces.