The concept of reference sample was put forward in the Guidance on CMC of Traditional Chinese Medicine Compound Preparations Developed from Catalogued Ancient Classical Prescriptions(Interim).The research on reference sample is a key link in the research and development of traditional Chinese medicine(TCM)compound prescriptions from catalogued ancient classical prescriptions(known as Category 3.1 TCM).This paper discusses the content of research on reference sample by analyzing the characteristics of Category 3.1 TCM and the purpose of research on reference sample.Furthermore,suggestions on the research of reference sample are proposed according to the development and evaluation practice of Category 3.1 TCM and research achievements of TCM regulatory science,aiming to provide reference for colleagues in this industry.

Fifteen previously undescribed 2-(2-phenylethyl)chromone dimers, along with two known analogues were isolated from Chinese agarwood (Aquilaria sinensis) by a LC-MS-guided fractionation procedure. Their structures were elucidated on the basis of spectroscopic and spectrometric data (1D and 2D NMR, IR, and HRESIMS). The isolated compounds exhibited significant inhibition of nitric oxide production in lipopolysaccharide-stimulated RAW264.7 cells with IC50 values in the range 0.6-37.1 mu M.

Activated B cells targeted to autoantigens proliferate and differentiate into antibody-secreting cells. Overproduced autoantibodies will give rise to autoimmune diseases. In this study, we investigated the inhibitory effects of GYF-21, an epoxide 2‑(2‑phenethyl)‑chromone derivative extracted from Chinese agarwood, on the survival, activation, proliferation, and differentiation of B cells for revealing its potential to treat autoimmune diseases related to B cell dysfunction. The results showed that GYF-21 slightly inhibited the survival, activation and proliferation of B cells stimulated by combination of anti-IgM, anti-CD40 and IL-4 while weakly up-regulated differentiation of B cells induced by combination of anti-CD40 and IL-4. In addition, GYF-21 intensively suppressed survival, activation, proliferation, and differentiation of B cells stimulated by B-cell activating factor (BAFF) which plays extremely important roles in autoantibody production and pathogenesis of autoimmune diseases. The mechanism study revealed that GYF-21 slightly down-regulated phosphorylation of NF-κB p65, Akt, STAT3, but up-regulated phosphorylation of Erk1/2 in B cells activated by anti-IgM, anti-CD40, IL-4 or their combinations. However, GYF-21 not only moderately down-regulated phosphorylation of NF-κB p65 and MAPK p38, but also intensively inhibited phosphorylation of Erk1/2 and Akt induced by BAFF. These data suggest the inhibitory effects of GYF-21 on the survival, activation, proliferation, and differentiation of B cells mainly via blocking BAFF activated signaling pathways, and its potential to be developed into therapeutic drug for autoimmune diseases, especially systemic lupus erythematosus (SLE).

Multiple sclerosis is a chronic inflammatory autoimmune disease of the central nervous system characterized by demyelinating plaques and axonal loss. Inhibition on over activation of innate and adaptive immunity provides a rationale strategy for treatment of multiple sclerosis. In the present study, we investigated the inhibitory effects of GYF-21, an epoxide 2-(2-phenethyl)-chromone derivative isolated from Chinese agarwood, on innate and adaptive immunity for revealing its potential to treat multiple sclerosis. The results showed that GYF-21 markedly inhibited the activation of microglia, and dendritic cells as well as neutrophils, all of which play important roles in innate immunity. Furthermore, GYF-21 significantly suppressed adaptive immunity via inhibiting the differentiation of naive CD4+ T cells into T helper 1 (Th1) and T helper 17 (Th17) cells, and suppressing the activation, proliferation, and IFN-γ secretion of CD8+ T cells. The mechanism study showed that GYF-21 evidently inhibited the activation of STAT1/3 and NF-κB signaling pathways in microglia. In conclusion, we demonstrated that GYF-21 can significantly inhibit innate and adaptive immunity via suppressing STAT1/3 and NF-κB signaling pathways, and has potential to be developed into therapeutic drug for multiple sclerosis.

Five new 2-(2-phenylethyl)chromone derivatives (1-5), along with eleven known compounds (6-16) were isolated from Chinese agarwood. Their structures were elucidated by spectroscopic data (NMR, UV, IR, and MS) analyses and comparison of their spectroscopic and physical data with the literature values. The absolute configurations of 2-4 were determined by electronic circular dichroism (ECD) calculations. Compounds 2-4, 11, 12, and 15 exhibited significant inhibition of nitric oxide production in lipopolysaccharide-stimulated RAW 264.7 cells with IC50 values in the range 1.6-7.3μM.

GYF-17, a 2-(2-phenethyl)-chromone derivative, was isolated from agarwood and showed superior activity of inhibiting NO production of RAW264.7 cells induced by LPS in our preliminary pharmacodynamic screening. In order to develop novel therapeutic drug for acute and chronic inflammatory disorders, the anti-inflammatory activity and underlying mechanism of GYF-17 were investigated in LPS-induced RAW264.7 cells. The results showed that GYF-17 could reduce LPS-induced expression of iNOS and then result in the decrement of NO production. More meaningful, the expression and secretion of key pro-inflammatory factors, including TNF-α, IL-6 and IL-1β, were intensively inhibited by GYF-17. Furthermore, GYF-17 also down regulated the expression of COX2 and the production of PGE2 which plays important role in causing algesthesia during inflammatory response. In mechanism study, GYF-17 selectively suppressed phosphorylation of STAT1/3 and ERK1/2 during the activation of NF-κB, MAPK and STAT signaling pathways induced by LPS. Collectively, GYF-17 can intensively suppress the production of LPS-induced inflammatory mediators in RAW264.7 cells by inhibiting STAT1/3 and ERK1/2 signaling pathways and thereby shows great potential to be developed into therapeutic drug for inflammatory diseases.

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

目的 建立沉香药材的HPLC-DAD特征图谱.方法 采用Diamonsil C18色谱柱(4.6 mm×250 mm,5μm),检测波长252 nm,柱温30℃,流动相为乙腈-0.1％甲酸水溶液,梯度洗脱,流速0.7 mL·min-,对23个批次沉香药材进行分析,并利用《中药色谱指纹图谱相似度评价系统》2004A进行数据处理.结果 通过多点校正及自动匹配,共确定了17个共有峰.通过与标准品比对,确证了其中的12个色谱峰.综合各批次沉香样品的差异、各成分含量及分离度,将其中的9个色谱峰设定为沉香药材的特征峰.以色谱峰1(沉香四醇)为参照,其他8个色谱峰的相对保留时间分别为1.033 6、1.219 3、1.248 6、1.783 3、1.891 5、1.918 4、2.404 6和2.458 2.结论 该方法符合方法学验证要求,可用于沉香药材的质量控制.

Ten new labdane diterpenoids, lagopsins A-H (1-3, 5, 7-10) and 15-epi-lagopsins C and D (4, 6), together with five known labdane diterpenoids (11-15), were isolated from the whole plants of Lagopsis supina. The absolute configuration of lagopsin A (1) was determined by single-crystal X-ray crystallographic analysis. Compounds 7, 9, 13, and 15 exhibited moderate inhibition of nitric oxide production stimulated by lipopolysaccharide in BV-2 microglial cells with IC50 values in the range 14.9-34.9 μM.

Six new polyoxygenated triterpenoids, cannabifolins A-F (1-6), and eight known triterpenoids, 7-14, were isolated from the leaves of Vitex negundo var. cannabifolia. The absolute configuration of cannabifolin A (1) was determined by single-crystal X-ray crystallographic analysis. Compounds 1 and 2 represent a class of rare natural pentacyclic triterpenoids bearing cis-fused C/D rings and are the first examples of 12,19-epoxy ursane- and oleanane-type triterpenoids. Compounds 3, 7, 8, and 14 exhibited inhibition of nitric oxide production in lipopolysaccharide-induced RAW 264.7 macrophages with IC50 values in the range 24.9-40.5 μM.

Four new lignanamides, melongenamides A–D (1–4), together with six known ones (5–10), were isolated from the roots of Solanum melongena L. Their structures were elucidated on the basis of 1D and 2D NMR experiments and by comparison of their spectroscopic and physical data with the literature values. Compounds 2–8 exhibited inhibitions of nitric oxide production in lipopolysaccharide-induced RAW 264.7 macrophages with IC50 values ranging from 16.2 to 58.5μM.

Objective To study the phenolic constituents of Draconis Resina.Methods The compounds were isolated and purified by silica gel and sephadex LH-20 column chromatography,and their structures were identified by physiochemical properties and MS and NMR spectroscopic data.Results Fourteen compounds were isolated from the ethyl acetate extract of Draconis Resina and identified as 4′-hydroxy-1′,4″-dimethoxychalcane(1),7-hydroxy-5,4′-dimethoxy-2-arylbenzofuran(2),pterostilbene(3),3,4′-dihydroxy-5-methoxystilbene(4),5,7,4′-trihydroxyflavanone(5),pinocembrin(6),7-hydroxyflavanone(7),liquiritigenin(8),methyl 4-hydroxybenzoate(9),methyl 4-hydroxy-3-methoxybenzoate(10),ethyl 4-hydroxy-3-methoxybenzoate(11),2,4-dihydroxy acetophenone(12),3,4-dihydroxyallybenzene(13),and β-sitosterol(14).Conclusion Compound 1 is a new natural product.Compound 2 is firstly obtained from the plants of Liliaceae.Compounds 5 and 9—12 are firstly isolated from the plants of Dracaena Vand.ex L.,and compounds 6 and 7 are isolated from Dracaena cochinchinensis for the first time.

This study was aimed to establish a quantitative method for the determination of agarotetrol in agarwood to control its quality. The HPLC analysis was performed on a Diamonsil C18 column (4.6 mm í 250 mm, 5 μm), eluted with a mobile phase of water with 0.1% formic acid and acetonitrile in gradient mode with the flow rate of 0.7 mL·min-1. The detection wavelength was set at 252 nm. The column temperature was 30oC. The results showed that the separation of agarotetrol and adjacent peaks were more than 1.5, which achieved a baseline separation. A good lin-earity (r = 0.999 8) was observed in the range of 2.0-125.0 μg·mL-1, with the average recovery of 102.75%. The a-garotetrol cannot be less than 0.15% based on the data of Agarwood samples. It was concluded that the method was accurate and reliable to determine the content of agarotetrol, which can be used for the quality control of agarwood.

A quantitative HPLC-DAD method was developed for simultaneous determination of N-trans-p-coumaroyloctopamine and N-trans-p-coumaroyltyramine in Solani Melongenae Radix from different cultivation regions in China The separation was performed on an Agilent Eclipse XDB C18 column (4.6 mm x 250 mm, 5 microm) at 30 degrees C with a gradient elution of methanol and 0.1% formic acid in water as mobile phase. The flow rate was set at 1.0 mL x min(-1) and the detection wavelength was 300 nm. The calibration curves of N-trans-p-coumaroyloctopamine and N-trans-p-coumaroyltyramine were linear over the ranges of 2.84-68.16, 3.10-74.40 mg x L(-1), and the average recoveries (n = 9) were 99.30% and 102.8%, respectively. The developed method was successfully applied for the analysis of sixteen samples from different cultivation regions in China, which indicated that the method is simple, rapid, accurate, and reliable for quality evaluation of Solani Melongenae Radix.

The modern pharmacology study has proved that Lagopsis supine has definite pharmacological effects in improving blood and lymph microcirculation,myocardial protection,anti-inflammatory and antioxidant. The study has found that labdane diterpenoid com-pound isolated from Lagopsis supine such as marrubin has many biological activities,such as the relaxation of blood vessels,heart pro-tection and antispasmodic and analgesic,etc. . The biological activity has the same effect with Lagopsis supine in promoting blood circu-lation to remove blood stasis,and anti-inflammatory. So study on labdane diterpenoid compound and its biological activity in Lagopsis supine has great significance in clarifying material efficacy base of Lagopsis supine. It is necessary for deeply study on the chemical con-stituents and pharmacological activities,and clarify its material efficacy basis and mechanism of action,which will provide a scientific basis for its further development and utilization.

A quantitative HPLC-DAD method was developed for simultaneous determination of N-trans-p-coumaroyloctopamine and N-trans-p-coumaroyltyramine in Solani Melongenae Radix from different cultivation regions in China The separation was performed on an Agilent Eclipse XDB C18 column (4.6 mm x 250 mm, 5 microm) at 30 degrees C with a gradient elution of methanol and 0.1% formic acid in water as mobile phase. The flow rate was set at 1.0 mL x min(-1) and the detection wavelength was 300 nm. The calibration curves of N-trans-p-coumaroyloctopamine and N-trans-p-coumaroyltyramine were linear over the ranges of 2.84-68.16, 3.10-74.40 mg x L(-1), and the average recoveries (n = 9) were 99.30% and 102.8%, respectively. The developed method was successfully applied for the analysis of sixteen samples from different cultivation regions in China, which indicated that the method is simple, rapid, accurate, and reliable for quality evaluation of Solani Melongenae Radix.

茄是一种药食两用植物,富含咖啡酰奎宁酸酯衍生物、黄酮类、生物碱类、甾体皂苷类等多种化学成分,具有抗炎、镇痛、抗氧化、调血脂、降血糖和抗肿瘤等多种生物活性。综述了国内外对茄的化学成分及药理作用研究进展,并对茄的开发利用前景进行展望,为进一步合理开发和综合利用茄的药用资源提供有益参考。

Objective To study the chemical constituents of the leaves of Exochorda serratifolia S.Moore. Methods Isolation and purification were carried out on the chromatography of silica gel and Sephadex LH-20.Their structures were elucidated on basis of physicochemical properties and spectral data. Results Six compounds were isolated and identified as apigenin( 1),luteolin( 2),quercetin( 3),quercetin-3-O-β-D-glucopyranoside( 4),apigenin-7-O-β-D-glucopyranoside( 5)and apigenin-7-O-β-D-neospheroside( 6). Conclusions Compounds 16 are isolated from this plant for the first time.