栀子环烯醚萜类通过犬血脑屏障后成分的检测

目的:通过对栀子环烯醚萜类进入脑脊液的移行成分分析,阐明栀子治疗中枢神经系统疾病潜在的活性成分。方法:给予犬静脉注射栀子环烯醚萜类成分,并采集3个不同时间点的脑脊液,通过液相色谱-质谱联用(LC-MS)技术检测并鉴定脑脊液中的栀子环烯醚萜类成分,通过MS和核磁共振(NMR)检测余下的栀子环烯醚萜成分。结果:在脑脊液中存在3种栀子环烯醚萜类成分。利用LC-MS分析确认其中1种成分为栀子苷;而采用MS和NMR数据确证的其他2种栀子环烯醚萜类成分分别为去乙酰基车叶草苷酸甲酯和京尼平-β-D-龙胆双糖苷。结论:栀子环烯醚萜类成分中栀子苷、去乙酰基车叶草苷酸甲酯和京尼平-β-D-龙胆双糖苷能够通过血脑屏障进入脑脊液,其透过的机制和药理作用还有待进一步研究。     

用二阶导数光谱法测定栀子中总环烯醚萜苷的含量

目的：建立测定栀子中总环烯醚萜苷含量的二阶导数光谱法,并用该方法测定不同产地栀子中总环烯醚萜苷的含量。方法：采用二阶导数光谱法在263nm波长处测定栀子中总环烯醚萜苷的含量。结果：栀子苷在4.32～21.60μg/ml范围内呈良好线性关系;其回归方程为A=2.986×10-5c-1.833×10-5（r=0.9996）;回收率为（98.86±2.39）%（n=5）,精密度、重现性和稳定性良好。结论：本方法操作简单、准确,可用于测定栀子中总环烯醚萜苷的含量。     

用LC-MS/MS法同时测定栀子中3种环烯醚萜苷类成分的含量

目的 建立同时测定栀子中3种环烯醚萜苷类成分含量的方法。方法 采用液相色谱-串联质谱（LC-MS/MS）法。色谱条件：Dikma Diamonsil^® C₁₈柱（100 mm×4.6 mm,5 μm）;流动相为0.1%乙酸水（A）-0.1%乙酸乙腈（B）,梯度洗脱;流速为0.4 ml/min;柱温40℃;进样量2 μl。质谱条件：电喷雾离子化电离源（ESI）,正/负离子检测,雾化气流量3 L/min,干燥气流量15 L/min,脱溶剂管温度240℃,加热块温度400℃,碰撞气压力230 kPa,以多反应监测模式（MRM）配对离子方式进行定量,山栀苷、京尼平龙胆双糖苷、栀子苷选择的离子对质荷比分别为m/z 391.10→149.30,m/z 573.40→365.05,m/z 447.30→225.15。结果 回归方程为：山栀苷Y=243.810X-289.957,r=0.999 9;京尼平龙胆双糖苷Y=137.125X+2 092.76,r=0.999 6;栀子苷Y=2 030.32X+823 213,r=0.999 8;线性范围分别为10.76~2 152 ng/ml、516~4 128 ng/ml、2 000~20 000 ng/ml。精密度、稳定性、重复性和加样回收率试验结果均符合要求。结论 此方法可快速、准确、灵敏地测定栀子中3种环烯醚萜苷类成分的含量,为栀子的质量控制提供依据。     

基于偏最小二乘法关联分析栀子不同炮制品化学成分与肝肾毒性

目的 基于偏最小二乘回归法（PLS）研究栀子不同炮制品化学成分与肝肾毒性的关联度。方法 采用超高效液相色谱法测定生栀子、炒栀子、姜栀子、焦栀子、栀子炭不同炮制品中栀子苷、京尼平龙胆双糖苷、栀子苷酸、去乙酰车叶草酸甲酯、西红花苷I和西红花苷Ⅱ 6种化学成分的含量,栀子不同炮制品水提液（7.5 g/kg）连续3 d大鼠ig给药,测定各组大鼠血清丙氨酸氨基转移酶（ALT）、天冬氨酸氨基转移酶（AST）、总胆红素（TBIL）、血清肌酐（CREA）、尿素氮（BUN）的含量,使用Origin 9.1软件中的PLS算法分析栀子不同炮制品化学成分与肝肾毒性的关联度。结果 栀子炮制后栀子苷、西红花苷I和西红花苷Ⅱ的含量不同程度的降低,京尼平龙胆双糖苷、去乙酰车叶草酸甲酯和栀子苷酸含量在部分炮制品中升高;栀子及炮制品对正常大鼠可造成不同程度的肝、肾损伤（生栀子>炒栀子>姜栀子>焦栀子>栀子炭）;PLS分析表明6种主要化学成分中栀子苷与西红花苷I的变量重要性值均超过0.8。结论 栀子苷与西红花苷I可能是栀子肝肾毒性的物质基础,通过炮制降低栀子肝肾毒性的作用可能与炮制后栀子苷与西红花苷I含量降低有关。     

一测多评法测定茵栀黄颗粒中4个环烯醚萜苷类成分

目的 建立同时测定茵栀黄颗粒中栀子苷、山栀苷、去乙酰车叶草苷酸甲酯和京尼平-1-β-D-龙胆二糖苷的一测多评法,验证该方法在茵栀黄颗粒质量控制应用中的科学性和可行性。方法 采用高效液相色谱法,以栀子苷为内参物,建立该成分与山栀苷、去乙酰车叶草苷酸甲酯和京尼平-1-β-D-龙胆二糖苷的相对校正因子,利用相对校正因子来计算各成分的质量分数,同时用外标法测定茵栀黄颗粒中栀子苷等4个成分的质量分数,对一测多评的计算值和外标法实测值进行比较,验证一测多评法在茵栀黄颗粒中应用的科学性和准确性。结果 各相对校正因子重复性良好,一测多评法测定结果与外标法测定结果无显著差异。结论 在缺少对照品的情况下,以栀子苷为内标同时测定栀子苷、山栀苷、去乙酰车叶草苷酸甲酯和京尼平-1-β-D-龙胆二糖苷的一测多评法可用于茵栀黄颗粒的定量分析。     

独一味总环烯醚萜苷分离纯化工艺的优化

目的 优化独一味总环烯醚萜苷的制备工艺,获取纯度相对较高的总环烯醚萜苷。方法 以甲醇-水为流动相,梯度洗脱方式建立分离分析独一味总环烯醚萜苷的高效液相色谱方法,实现各组分的最佳分离,统计、记录其三维吸收图谱,并结合紫外全波长扫描,对前期制备的独一味总环烯醚萜苷中影响纯度的杂质特征进行分析,根据杂质特性优化大孔树脂结合聚酰胺柱制备过程,紫外实时监测,剔除杂质,产品溶液经冷冻干燥获得冻干粉,并以HPLC对比前后制备工艺产品成分差异。结果 工艺优化前产品中环烯醚萜苷含量为69.06%,优化后含量为90.60%,含量提升21.54%;本次制备总产率为16.70%（以水提取物的质量为参照）,总环烯醚萜苷转移率为74.72%（相对于水提取物中总环烯醚萜苷的质量）。结论 优化过程简单,操作步骤可控,易于实现,纯化效果显著。     

独一味与糙苏中环烯醚萜苷类成分的比较

目的 比较独一味与糙苏中的环烯醚萜苷类成分.方法 采用TLC法鉴别独一味与糙苏药材中的环烯醚萜苷类成分,建立HPLC法测定其中的8一乙酰氧基山栀子苷甲酯的含量.结果 糙苏及独一味均含有大量的环烯醚萜苷类成分,两者根部具有十分相似的薄层色谱图、地上部分及根部中8-乙酰氧基山栀子苷甲酯的含量分别为17.41、0.5、6.81、8.50 mg·g-1.结论 独一味根与糙苏根中含有相近的环烯醚萜苷类成分.     

HPLC法测定鸡矢藤药材中环烯醚萜苷含量

目的:采用高效液相色谱和二极管阵列检测器法(HPLC-DAD)同时测定鸡矢藤药材中3种主要环烯醚萜苷类成分的含量,研究不同产地鸡矢藤药材中环烯醚萜苷的含量.方法:色谱分析采用Shim-pack VP-ODS C18分析柱,0.1%的甲酸(A)和乙腈(B)为流动相进行梯度洗脱,检测波长:240nm.结果:3个环烯醚萜苷[鸡矢藤苷酸(1)、鸡矢藤苷(2)、鸡矢藤苷酸甲酯(3)]在标准曲线内均有较好的线性(r2>0.9999),且该方法具有良好的精密度,灵敏度,重复性和准确度;应用所建立的方法同时测定了8批鸡矢藤药材中三个环烯醚萜苷的含量.结论:本文首次报道建立HPLC-DAD方法同时测定鸡矢藤中主要环烯醚萜苷类成分含量,该方法简单、快速、可靠,适用于鸡矢藤药材及其制剂的质量控制.     

巴戟天环烯醚萜苷类成分含量测定和提取方法的研究

目的 建立测定巴戟天环烯醚萜苷类成分含量的方法,并研究其最佳提取方法。方法 以巴戟天环烯醚萜苷类成分水晶兰苷、去乙酰基车叶草苷酸、车叶草苷酸和车叶草苷为对照品,采用HPLC法进行含量测定。色谱柱为艾杰尔Venusil MP C_l8柱（250 mm ×4.6 mm, 5 μm）,流动相为乙腈（A）-0.2%磷酸+0.01 mol/L磷酸氢二钠缓冲盐（B）梯度洗脱（0~12 min,1%~2% A;12~30 min,2%~25% A）,检测波长为235 nm,流速为1.0 ml/min,柱温为25 ℃,进样量为20 μl。采用单因素考察和正交试验优化巴戟天环烯醚萜苷类成分的提取方法。结果 水晶兰苷、去乙酰车叶草苷酸、车叶草苷酸和车叶草苷在0.375~12、0.13~4.16、0.016~0.516和0.012~0.384 μg范围内,线性关系良好;重复性、精密度、加样回收率和稳定性试验结果均符合要求。优化的巴戟天环烯醚萜苷类成分的最佳提取方法为：巴戟天药材用16倍10%乙醇浸泡9 h,渗漉提取,流速为0.8 BV/h。结论 此法可准确、灵敏地测定巴戟天环烯醚萜苷类成分的含量,并可使该类成分得到充分提取。     

HPLC同时测定栀子药材中栀子苷和西红花苷-1的含量

目的同时测定10批栀子药材中栀子苷和西红花苷-1的含量。方法采用RP-HPLC法,ShimpackVP-ODS柱,乙腈-水梯度洗脱,检测波长238nm(0～20min,检测环烯醚萜苷类)、440nm(20～60min,检测西红花苷类)。结果和结论该方法简便、准确、重复性好,可同时测定栀子中不同检测波长的两大类有效成分。     

多波长高效液相色谱法同时测定栀子中的三类成分

目的同时测定栀子中3类有效组分，9个成分（栀子酸、栀子苷、异栀子苷、京尼平龙胆二糖苷、绿原酸、藏红花酸、3种藏红花素）的含量。方法紫外-可见三波长同时检测的高效液相色谱法：色谱柱为Phenomenex Luna C₁₈柱（250 mm×4.6 mm ID，5 μm）；流动相为(A)0.3％甲酸水溶液, (B)甲醇-乙腈（9∶1）；流速为0.8 mL·min^-1；柱温为35 ℃；检测波长为 240 nm(栀子酸、栀子苷、异栀子苷、京尼平龙胆二糖苷), 330 nm(绿原酸)和440 nm(藏红花酸和3种藏红花素)；线性梯度洗脱。结果建立了同时对栀子中的9个成分进行定量的测定方法，并将此方法用于5个产地栀子各成分的测定。结论为中药材栀子提供了更合理、可靠的质控方法。     

Metabolism and pharmacokinetics of genipin and geniposide in rats

Geniposide, an iridoid glucoside, is a major constituent in the fruits of Gardenia jasminoides (Gardenia fruits), a popular Chinese herb. Genipin, the aglycone of geniposide, is used to prepare blue colorants in food industry and also a crosslinking reagent for biological tissue fixation. In this study, we investigated the metabolism and pharmacokinetics of genipin and geniposide in rats. Blood samples were withdrawn via cardiopuncture and the plasma samples were assayed by HPLC method before and after hydrolysis with sulfatase and beta-glucuronidase. The results indicated that after oral administration of genipin or Gardenia fruit decoction, genipin sulfate was a major metabolite in the bloodstream, whereas the parent forms of genipin and geniposide were not detected. Importantly, oral administration of 200mg/kg of genipin resulted in a mortality of 78% (7/9) in rats.     

Gardenia jasminoides Ellis ethanol extract and its constituents reduce the risks of gastritis and reverse gastric lesions in rats

In this study we investigated the effects of Gardenia jasminoides Ellis (GJE) extract and its constituents, such as ursolic acid and genipin, on gastritis in rats and the growth of human gastric cancer cells. The GJE extract, ursolic acid and genipin showed the acid-neutralizing capacities, the antioxidant activities, and the inhibitory effects on the growth of Helicobacter pylori (H. pylori), which are almost equivalent to positive control compounds. In addition, the GJE extract and ursolic acid had cytotoxic activity against AGS and SUN638 gastric cancer cells. The genipin and ursolic acid inhibited significant HCl/ethanol-induced gastric lesions. Taken together, GJE extract and its constituents might have antigastritic activities, associated with the antioxidant activities, acid-neutralizing capacities, and anti-H. pylori action. Also, we could suggest that genipin and ursolic acid may be useful for the treatment and/or protection of gastritis.     

Chemistry and bioactivity of Gardenia jasminoides

Gardenia jasminoides, grown in multiple regions in China, was commonly used as a natural yellow dye but has been one of the popular traditional Chinese medicines since the discovery of its biological property a few decades ago. It has been reported that G. jasminoides possess multiple biological activities, such as antioxidant properties, hypoglycemic effect, inhibition of inflammation, antidepression activity, and improved sleeping quality. In this review, our aim was to have a comprehensive summary of its phytochemistry including the extraction, isolation, and characterization of volatiles and bioactive molecules in G. jasminoides, focusing on the two major phytochemicals, genipin and crocin, which possess potent medicinal properties. Furthermore, this study attempted to establish a structure–activity relationship between the two major series of molecules with two pharmcophores and their biological activities, which would serve further exploration of the properties of phytocompounds in G. jasminoides as potential functional foods and medicines.     

栀子化学成分的研究

由中药梔子中分离得D-甘露醇,β-谷甾醇,二十九烷和两种尚未鉴定的色素成分。     

A rubrofusarin gentiobioside isomer from roastedCassia tora

From the roasted seeds ofCassia tora L., a new naphthopyrone glycoside was isolated and characterized as 10-[(β-D-glucopyranosyl-(1→6)-O-β-D-glucopyranosyl)oxyl-5-hydroxy-8-methoxy-2-methyl-4H-naphtho [1,2-b]pyran-4-one(isorubrofusarin gentiobioside). Along with isorubrofusarin gentiobioside, alaternin and adenosine were isolated and identified.     

Genipin Inhibits RANKL-Induced Osteoclast Differentiation Through Proteasome-Mediated Degradation of c-Fos Protein and Suppression of NF-κB Activation

People over the age of 50 are at risk of osteoporotic fracture, which may lead to increased morbidity and mortality. Osteoclasts are responsible for bone resorption in bone-related disorders. Genipin is a well-known geniposide aglycon derived from Gardenia jasminoides, which has long been used in oriental medicine for controlling diverse conditions such as inflammation and infection. We aimed to evaluate the effects of genipin on RANKL-induced osteoclast differentiation and its mechanism of action. Genipin dose-dependently inhibited early stage RANKL-induced osteoclast differentiation in bone marrow macrophages (BMMs) during culture. Genipin inhibited RANKL-induced IκB degradation and suppressed the mRNA expression of osteoclastic markers such as NFATc1, TRAP, and OSCAR in RANKL-treated BMMs, but did not affect c-Fos mRNA expression. Interestingly, genipin markedly inhibited c-Fos protein expression in BMMs, which was reversed in the presence of the proteosome inhibitor MG-132. Furthermore, genipin inhibited RANKL-mediated osteoclast differentiation, which was also rescued by overexpression of c-Fos and NFATc1 in BMMs. Taken together, our findings indicate that genipin down-regulated RANKL-induced osteoclast differentiation through inhibition of c-Fos protein proteolysis as well as inhibition of IκB degradation. Our findings indicate that genipin could be a useful drug candidate that lacks toxic side effects for the treatment of osteoporosis.     

HPLC测定不同品种酸模中蒽醌类成分的含量

目的建立酸模药材中蒽醌类成分含量测定的方法;并比较不同品种不同产地酸模药材中蒽醌类成分的含量,为确定酸模药材来源提供依据。方法采用HPLC测定酸模药材中蒽醌类成分的含量。结果比较不同品种不同产地13批样品的测定结果,酸模中蒽醌类成分的含量最高,大黄素、大黄酚、大黄素甲醚3者总量,酸模约为0.95%～2.12%,齿果酸模约0.24%～0.39%,长刺酸模约为0.04%～0.15%,小酸模约为0.39%～0.46%。结论建立的蒽醌类成分含量测定方法准确可靠;不同品种酸模中蒽醌含量差异较大。