经典名方桃核承气汤的UPLC指纹图谱及多指标成分含量测定研究

目的 通过建立UPLC指纹图谱及多指标成分含量测定方法,构建经典名方桃核承气汤（Taohe Chengqi Decoction,TCD）的质量体系,研究TCD基准样品量值传递规律。方法 遵照古籍记载并结合工艺考察,制备不同产地的15批次TCD基准样品,采用UPLC法建立基准样品指纹图谱,使用中药色谱指纹图谱相似度评价软件（2012版）进行相似度评价,结合UPLC-Q-Exactive Orbitrap-MS技术全面分析基准样品化学成分,同时测定样品中指标成分（苦杏仁苷、桂皮醛、肉桂酸、甘草酸、游离型蒽醌、总蒽醌、结合蒽醌）的含量。结果 建立了15批TCD基准样品的UPLC指纹图谱,与对照指纹图谱比较相似度≥0.90,通过对照品确认、高分辨质谱数据分析及文献比对,共鉴定出80个化学成分,共归属26个指纹峰,鉴定了17个色谱峰。15批TCD基准样品中苦杏仁苷、桂皮醛、肉桂酸、甘草酸、游离型蒽醌、总蒽醌、结合蒽醌的质量分数分别为0.29%～0.58%、0.011%～0.032%、0.05%～0.13%、0.48%～1.04%、0.20%～0.30%、0.42%～0.66%、0.19%～0.37%,饮片到基准样品的转移率分别为31.49%～60.78%、0.43%～2.67%、51.61%～76.99%、26.79%～49.88%、16.01%～32.65%、9.66%～19.07%、6.97%～19.48%;出膏率为19.55%～22.92%,传递率为80.98%～99.34%。结论 所建立的UPLC指纹图谱及多指标成分含量测定分析方法快速简便,结合基准样品的量值传递过程分析,可为后续制剂的开发和质量控制提供理论依据。     

薄层扫描法测定肉桂中桂皮醛的含量

用氯仿提取,薄层扫描法直接测定药材中桂皮醛的含量,可作为评介肉桂质量的指标。     

Medicinal Plants In Khao Kho District,Phetchabun Province,Thailand

A survey on the utilization of medicinal plants used by Thai people at Khao Kho District, Petchabun Province was carried out by interviewing herbalists followed by collecting plant specimens and identifying the specimens. In addition, the plant specimens were compared with the authentic specimens at two herbaria: the Bangkok Herbarium, Botany Section, Botany and Weed Science Division, Department of Agriculture, Ministry of Agriculture, and the Forest Herbarium, Royal Forest Department, Ministry of Agriculture. Fifty-nine kinds of medicinal plants belonging to 32 families are reported, from which 12 kinds are newly recorded as medicinal plants. They were found belonging to 47 dicots, eight monocots, one gymnosperm, two ferns and one lichen. Forty-one kinds are used in combination with other medicinal plants whereas the other 17 kinds are used as a single remedy.     

双标多测法在柏子养心丸5个成分含量测定中的应用

目的:建立柏子养心丸中阿魏酸、桂皮醛、五味子醇甲、五味子甲素及五味子乙素5个成分的双标多测法,验证该方法在柏子养心丸质量评价中应用的准确性和可行性。方法:采用HPLC法,以乙腈为流动相A,0.1%醋酸溶液为流动相B,梯度洗脱(0～70 min,20%A;70～85 min,20%A→80%A),流速为1 mL·min-1,检测波长335 nm(0～31 min)、285 nm(31～52.5 min)、215 nm(52.5～85 min),柱温35℃。采用6根不同型号的C18色谱柱,测定柏子养心丸5个成分的实际保留时间,计算各成分在各色谱柱保留时间的平均值,得到各成分的标准保留时间,选取阿魏酸(峰1)、五味子乙素(峰5)作为双标化合物,使用双标线性校正法准确定位各成分色谱峰,预测成分在未知色谱柱的保留时间并进行方法学验证。以阿魏酸为参照物,计算其余各成分的相对校正因子,对各成分进行定量。结果:双标线性校正法能够准确地预测待测组分在未知色谱柱上的保留时间;桂皮醛、五味子醇甲、五味子甲素、五味子乙素相对于阿魏酸的相对校正因子分别为0.2644、0.4062、0.3772、0.3994,其...     

多指标正交试验优选苓桂术甘颗粒水提工艺

目的 优选苓桂术甘颗粒的水提工艺。方法 采用正交试验对水提工艺进行优化,以桂皮醛转移率、甘草酸转移率和干膏得率为评价指标,考察加水量、煎煮时间、煎煮次数对提取工艺的影响。结果 最佳提取工艺为加8倍量水,提取3次,每次煎煮1 h。结论 多指标加权考察水提工艺,既符合中药复方的复杂性,又能合理反映水提效果。该水提工艺设计合理,可为苓桂术甘颗粒的研制提供理论和试验基础。     

肉桂中4种成分近红外定量分析模型的建立

目的:采用近红外光谱法(NIR,near infrared spectroscopy)结合高效液相色谱法(HPLC,high performance liquid chromatography)建立肉桂饮片的快速评价方法。方法:收集不同产地的肉桂86批,采用HPLC法测定不同批次肉桂饮片中香豆素、肉桂醇、肉桂酸、肉桂醛的含量,同时采集不同批次肉桂的NIR光谱。以NIR光谱为自变量,以香豆素、肉桂醇、肉桂酸、肉桂醛的含量为因变量,采用偏最小二乘法(PLS,partial least squares)建立肉桂中4种成分的定量分析模型,并以校正集进行验证。结果:肉桂饮片中香豆素、肉桂醇、肉桂酸、肉桂醛近红外定量分析模型的相关系数(r)依次为0.952 8,0.977 7,0.961 9,0.992 2,校正集预测误差均方根(RMSEC)依次为0.012 2,0.006 1,0.004 3,0.82 g·g^-1,均方根误差(RMSECV)依次为0.015 8,0.011 2,0.002 0,1.481 1 g·g^-1,测试集预测误差均方根(RMSEP)依次为0.017 8,0.010 3,0.005 6,1.63 g·g^-1。结论:该实验所建立的肉桂饮片中香豆素、肉桂醇、肉桂酸、肉桂醛4种有效成分的近红外定量分析模型具有较好的准确性,可用于这4种成分的快速同步测定,为实现肉桂饮片质量的快速评价提供依据。     

剑叶三宝木的化学成分研究

目的研究剑叶三宝木Trigonostemonxyphophylloides的化学成分。方法运用硅胶柱色谱、半制备高效液相色谱等方法进行分离纯化,结合现代波谱技术及理化常数鉴定结构。结果从剑叶三宝木中分离得到了12个化合物,包括8个二萜类、2个香豆素类、1个苯基丙烯衍生物、1个木脂素类,分别鉴定为补骨脂素(1)、异补骨脂素(2)、3,4,5-三甲氧基肉桂醛(3)、domohinone(4)、12-hydroxy-13-methylpodocarpa-9,11,13-trien-3-one(5)、sonderianol(6)、trigonostemone(7)、trigoxyphin N(8)、trigonochinene E(9)、trigoxyphin A(10)、trigoxyphin Q(11)、2,6,2′,6′-四甲氧基-4,4′-双(2,3-环氧-1-羟丙基)联苯(12)。结论化合物1～5为首次从该属植物中分离得到,化合物6、7、9、11、12为首次从该种植物中分离得到。     

Cinnamaldehyde up-regulates the mRNA expression level of TRPV1 receptor potential ion channel protein and its function in primary rat DRG neurons in vitro

Cinnamaldehyde (1) is a pharmacologically active ingredient isolated from cassia twig (Ramulus Cinnamomi), which is commonly used in herbal remedies to treat fever-related diseases. Both TRPV1 and TRPM8 ion channel proteins are abundantly expressed in sensory neurons, and are assumed to act as a thermosensor, with the former mediating the feeling of warmth and the latter the feeling of cold in the body. Both of them have recently been reported to be involved in thermoregulation. The purpose of this paper is to further uncover the antipyretic mechanisms of 1 by investigating its effects on the mRNA expression levels and functions of both TRPV1 and TRPM8. The results showed that 1 could up-regulate the mRNA expression levels of TRPV1 at both 37 and 39°C, and its calcium-mediating function was significantly increased at 39°C, all of which could not be blocked by pretreatment of the neuronal cells with ruthenium red, a general transient receptor potential (TRP) blocker, indicating that the action of 1 was achieved through a non-TRPA1 channel pathway. In conclusion, the findings in our in vitro studies might account for part of the peripheral molecular mechanisms for the antipyretic action of 1.     

桂枝茯苓方的化学成分、药理作用及质量标志物(Q-marker)的预测分析

桂枝茯苓方为经典的活血化瘀方,具有改善血液流变性、调节内分泌、抗炎、抗肿瘤、镇痛等作用。古代用于治疗妇人妊娠下血、行经腹痛、产后恶露不尽等症。现代临床其常用于治疗妇科疾病,如子宫肌瘤、卵巢囊肿、痛经、子宫内膜异位症等。对桂枝茯苓方近年来的化学成分、药理作用、临床应用以及质量控制的研究进展进行综述,并在此基础上,基于中药质量标志物(Q-marker)的"五原则"对桂枝茯苓方的Q-marker进行预测分析,以期为桂枝茯苓方的质量控制研究提供参考。     

超声强化超临界流体萃取桂皮醛的工艺研究

目的对超声强化超临界流体(CO2)萃取肉桂中桂皮醛成分的工艺条件进行选择。方法采用超声超临界流体(CO2)萃取法,选取萃取温度、萃取压力、萃取时间和超声功率为因素,以桂皮醛为指标成份,采用正交试验对萃取方法进行优选。结果超临界萃取的最佳工艺条件为45℃,35 MPa,2 h,2 kW,桂皮醛平均提取率为18.76 mg/g。结论超声强化超临界技术提取肉桂挥发油中桂皮醛得率高于其他文献报道。该技术工艺合理,可行。