目的:考察小承气汤水煎液不同干燥方法制备得到的物质基准化学成分的差异,从物质基准化学成分的角度,为小承气汤颗粒剂工厂化制备确定最佳干燥方法提供依据.方法:采用HPLC指纹图谱方法,分别对水煎液及其在冷冻干燥、喷雾干燥、减压干燥和脉动真空干燥方法制得的小承气汤物质基准进行HPLC指纹图谱相似度等分析.结果:通过对4种干燥方法制得的样品与水煎液相似度的比较,发现干燥后的物质基准与水煎液相似度均达到0.9以上,相似度较好.水煎液及其物质基准的HPLC指纹图谱能够反映小承气汤水煎液浓缩干燥的整体化学成分轮廓,且脉动真空干燥更适合工厂化生产.结论:脉动真空干燥可作为小承气汤颗粒剂工厂化制备的干燥方法.

目的:采用HPLC对62批次大黄药材中的13个蒽醌类成分进行含量测定并对其HPLC指纹图谱进行相似度评价,为经典名方小承气汤物质基准研究提供合格的药材与饮片.方法:采用Diamonsil C18柱(150 mm×4.6 mm,5μm),以甲醇-0.1％磷酸水为流动相,梯度洗脱,流速1 mL/min;柱温为25℃;检测波长为254 nm.采用中药色谱指纹图谱相似度评价软件(2012版),对62个不同产地的大黄HPLC-FP进行相似度评价,并用SPSS 21软件对色谱数据进行聚类分析.结果:甘肃各产地的大黄药材含量相对稳定,相似度分析及聚类分析结果也表明甘肃各产区大黄药材相似度较高,四川、重庆及湖北产大黄药材含量测定结果接近,相似度及聚类分析可与甘肃及青海产大黄药材区分开来.结论:本含量测定方法简便、可靠,并可用于大黄药材的指纹图谱相似度评价;各批次药材含量测定结果均符合《中国药典》(2020版)大黄项下要求,可用于经典名方小承气汤物质基准研究.

目的 采用傅里叶变换红外光谱(FT-IR)和高效液相色谱(HPLC)方法对37批不同品种和产地的大黄药材进行分析.方法 分别采用FT-IR和HPLC测量37批大黄药材的红外光谱和液相指纹图谱,并对结果进行聚类分析.从每一产地中选择一批药材,分析红外原始光谱,并对原始光谱进行二阶导数处理,根据所得二阶导数光谱对各产地大黄进行分析;同时对HPLC指纹图谱进行相似度分析.结果 FT-IR和HPLC两种方法聚类分析结果基本一致.通过分析不同产地的大黄药材原始红外光谱特征峰能够区分各产地大黄品种,但无法区分其产地,而二阶导数特征峰有明显的位置、形态和强度上的差异,能够将不同产地大黄药材鉴别出来.HPLC指纹图谱相似度分析无法将其产地进行区分.结论 与HPLC指纹图谱相比,FT-IR能够更加全面的反映大黄药材的化学成分,并对其品种和产地进行区分.

目的:建立小承气汤物质基准的高效液相色谱法(HPLC)指纹图谱,结合化学模式识别方法对其质量进行分析与评价.方法:采用Diamonsil C18色谱柱(4.6 mm×150 mm,5 μm),流动相甲醇(A)-0.1％磷酸水溶液(B)梯度洗脱(0～60 min,20％～90％A;60～70min,90％～100％A),流速1 mL·min1,柱温25℃,检测波长254 nm.利用"中药色谱指纹图谱相似度评价系统"(2012版)软件对15批小承气汤物质基准的HPLC指纹图谱进行相似度评价,同时,采用聚类分析、主成分分析及正交偏最小二乘法-判别分析对指纹图谱数据进行分析,评价不同批次间小承气汤物质基准的质量差异,并找寻造成批间质量差异的主要化学成分.结果:建立了小承气汤物质基准的HPLC指纹图谱,确定了 31 个共有峰,并对各共有峰进行药材归属,通过与对照品比对指认了其中18个成分;15批小承气汤物质基准的HPLC指纹图谱与对照指纹图谱的相似度均＞0.92;3种化学模式识别方法均可将样品分为两类;筛选出了包括大黄酸,大黄酚-8-O-β-D-葡萄糖苷,芦荟大黄素-8-O-β-D-葡萄糖苷,番泻苷A,大黄酚-1-O-β-D-葡萄糖苷,大黄酸-8-O-葡萄糖苷在内的9种主要差异成分.结论:建立的指纹图谱分析方法灵敏度高、稳定性强、数据准确可靠,基本体现了小承气汤物质基准的整体化学成分特征,可为该经典名方复方制剂的质量标准建立提供依据.

Ethnopharmacological relevance: Fructus Aurantii (FA) is a Chinese herbal medicine commonly used in clinical practice to improve gastrointestinal motility, treat dyspepsia, and relieve constipation. More than 20 processing methods of FA have been recorded, among which FA stir-baked with bran is the earliest, most time consuming, and the most popular one. Raw FA has a strong ability to promote qi-moving and has middle-energizer-soothing effects; therefore, it is often used to relieve hypochondrium distension and pain, and to relax the stagnation of the liver Qi. FA stir-baked with bran is more effective in nourishing the stomach and curing indigestion. Aim of the study: In this study, the chemical composition and differences between raw FA and FA stir-baked with bran were systematically compared. The chemical components that increased after stir-baking FA and bran were separated and their pharmacodynamic characteristics were determined. Lastly, the processing mechanism of FA was further explained. Materials and methods: Twelve main chemicals in raw FA and FA stir-baked with bran were compared using high-performance liquid chromatography (HPLC). The main differential components were identified, separated, purified, and then analyzed using pharmacodynamic tests. The intestine-pushing test, in vitro smooth muscle test, and in vitro acetylcholinesterase (AchE) activity test in mice were performed to explain the mechanism of auraptene in improving gastrointestinal motility. Results: Using HPLC, the primary chemical that differed between raw FA and FA stir-baked with bran was identified as auraptene. The processed FA was extracted, separated, and purified to obtain pure auraptene. The intestine-pushing test in mice showed that low (0.6 mg.kg(-1)) and medium doses (1.2 mg.kg(-1)) of auraptene could promote peristalsis of the small intestine, whereas a high dose (2.4 mg.kg(-1)) inhibited peristalsis. In vitro studies on the smooth muscle of mice showed that a low dose of auraptene (0.2 mmol.L-1, 10-800 mu L) could promote contraction, whereas a high dose (0.2 mmol.L-1, >1000 mu L) had the opposite effect. Auraptene has a mechanism of action similar to that of the acetylcholinesterase inhibitor, neostigmine. Additionally, auraptene could inhibit AchE activity in vitro. Conclusions: Auraptene is the main chemical constituent that differs between raw FA and FA stir-baked with bran. Pharmacodynamic tests showed that auraptene has a cholinergic effect, by virtue of its role as an acetylcholinesterase inhibitor. Moreover, auraptene could dually regulate the gastrointestinal smooth muscle. Auraptene was present in low levels and its content varied in FA stir-baked with bran, depending on the origin and source of FA, and the treatment procedures it was subjected to. In the Chinese Pharmacopoeia, the recommended dose of FA stir-baked with bran is a low dose of 3-10 g, which effectively promotes small-intestinal peristalsis. The mechanism of action is attributed to an increase in the relative content of acetylcholine by the inhibition of AchE activity to promote gastrointestinal motility. The increased levels of auraptene in FA stir-baked with bran are the main reason and the primary purpose for the change in its medicinal properties. This technique, therefore, has potential to be used as one of the main processing mechanisms of raw FA.

小承气汤源自《伤寒论》,由大黄(酒洗)4两、厚朴(炙,去皮)2两、枳实(大者,炙)3枚组成,常用于治疗阳明腑实轻证,被收录于《古代经典名方目录(第一批)》,具有较高的临床应用价值.目前对小承气汤的化学成分、药理作用、临床应用等方面已有较多研究,但处方历史沿革不清、剂量换算不明,这些都对经典名方小承气汤的临床合理应用及其复方制剂的研发造成了一定的困难.笔者拟对小承气汤处方历史沿革、药味基原、饮片炮制方法、剂量换算和现代研究等方面进行综述,以明确该复方的历史脉络,为经典名方小承气汤的中医临床运用及其现代科学研究提供依据.

目的:探讨生态环境对枳壳活性成分形成和累积的影响.方法:采取高效液相色谱法分析了江西樟树、新干,重庆綦江、奉节、江津,湖南沅江、汉寿,浙江衢州等地区枳壳中12种活性成分的含量,利用世界气候数据库及中国土壤数据集获得气温、降水量、海拔等8个生态因子数据,采用典型相关分析等方法探讨生态环境因子对枳壳活性成分的影响.结果:通过对枳壳活性成分含量与生态因子进行典型相关分析,发现采摘期辐射与枳壳黄酮类成分橙皮苷、橘皮素和柚皮苷含量呈显著相关,说明在一定范围内,辐射影响枳壳黄酮类成分累积;而生长期降水量与枳壳香豆素类成分水合橘皮内酯含量呈显著相关,即适宜的降雨有利于水合橘皮内酯含量累积.结论:枳壳种植过程中通过对生长期降水量和采收期辐射的控制可调控枳壳活性成分含量.