高效液相色谱校正因子法测定苦碟子提取物中5种主要成分的含量

目的通过测定苦碟子提取物中咖啡酸、菊苣酸、木犀草素-7-O-β-D-葡萄糖苷-(1→6)-β-D-葡萄糖苷、芹菜素-7-O-β-D-葡萄糖醛酸苷与木犀草素-7-O-β-D-葡萄糖醛酸苷的校正因子,建立以1种对照品测定苦碟子提取物中5种主要成分的含量的方法。方法以Agilent TC-C18(250 mm×4.6 mm,5μm)为分析柱,柱温30℃,流动相为甲醇(A)-0.05%磷酸(B),梯度洗脱:0~10 min:30%A,10~30 min:30%~50%A,流速1.2 mL.min-1,检测波长350 nm。结果咖啡酸、菊苣酸、木犀草素-7-O-β-D-葡萄糖苷-(1→6)-β-D-葡萄糖苷、芹菜素-7-O-β-D-葡萄糖醛酸苷的校正因子分别为:1.129、0.873 3、1.320、1.129(RSD=1.6%~2.1%),苦碟子提取物中咖啡酸、菊苣酸、木犀草素-7-O-β-D-葡萄糖苷-(1→6)-β-D-葡萄糖苷、木犀草素-7-O-β-D-葡萄糖醛酸苷与芹菜素-7-O-β-D-葡萄糖醛酸苷的含量分别为4.2%、29.5%、6.5%、23.0%、5.0%。结论本法简便,灵敏,重现性好,可用于苦碟子提取物和制剂的定量分析及质量控制。     

HPLC法测定不同采收期香青兰中黄酮和酚酸类的含量北大核心CSCD

目的:测定不同时期采收的香青兰药材中黄酮类成分(木犀草素-7-O-β-D-葡萄糖醛酸苷、芹菜素-7-O-β-D-葡萄糖醛酸苷、香叶木素-7-O-β-D-葡萄糖醛酸苷和田蓟苷)和酚酸类成分(迷迭香酸)的含量,确定最佳采收期。方法:采用PurospherSTAR LP RP-18 endcapped(4.6 mm×250 mm,5μm)色谱柱,以乙腈(A)-0.5%甲酸水溶液(B)为流动相,梯度洗脱(0~30 min,17% A;30~60 min,17% A→28% A;60~75 min,28% A),流速1.0 mL·min^(-1),检测波长330 nm,柱温35℃。结果:木犀草素-7-O-β-D-葡萄糖醛酸苷、芹菜素-7-O-β-D-葡萄糖醛酸苷、迷迭香酸、香叶木素-7-O-β-D-葡萄糖醛酸苷、田蓟苷5种化学成分的分离效果良好,质量浓度在相应的范围内与峰面积有良好的线性关系,相关系数均大于0.999 5;平均加样回收率(n=6)为98.4%~99.5%(RSD<1.9%,n=6)。该方法应用于研究新疆吉木萨尔县产区不同采收期对香青兰药材中5种化学成分含量的影响,本试验在6月13日(种植后213 d)至8月6日(种植后270 d)内设置了8个采收期,发现木犀草素-7-O-β-D-葡萄糖醛酸苷等上述5种化学成分的含量与采收期(种植后天数)均呈二次或三次函数关系,随着采收期的推迟,含量先增后减。结论:该含量测定方法操作简单,重复性好,为确定香青兰药材适宜采收期提供依据。香青兰药材中木犀草素-7-O-β-D-葡萄糖醛酸苷等5种化学成分含量随采收期不同而异,其总量最大值出现在7月中上旬。     

HPLC-DAD法测定苦碟子中木犀草素7-O-β-D-葡萄糖苷、木犀草素7-O- β-D-葡萄糖醛酸苷和芹菜素7-O-β-D-葡萄糖醛酸苷

目的利用HPLC-DAD法建立苦碟子中木犀草素7-O-β-D-葡萄糖苷(LGCOP)、木犀草素7-O-β-D-葡萄糖醛酸苷(LGCRP)和芹菜素7-O-β-D-葡萄糖醛酸苷(AGCRP)的测定方法。方法 Diamonsil C18色谱柱(200 mm×4.6 mm,5μm);流动相为(0.05%甲酸–水)–(0.05%甲酸–乙腈);二元梯度洗脱:检测波长340 nm;体积流量1.0 mL/min;柱温35℃;进样量10μL。结果在选定色谱条件下线性关系良好(r≥0.999 9)。平均回收率分别为100.5%、100.1%、100.8%,RSD值分别为0.4%、0.3%、0.7%。结论该分析方法能简便、快速地测定苦碟子中黄酮类成分,可为评价不同产地、药用部位及采收期的药材提供科学依据。     

风轮菜中黄酮苷类化合物的结构鉴定

从风轮菜全草的乙醇提取物中分离并鉴定了3个黄酮苷类人工产物,分别为芹菜素-7-氧-β-D-吡喃葡萄糖醛酸丁酯（1）、木犀草素-7-氧-β-D-吡喃葡萄糖醛酸丁酯（2）和柚皮素-7-氧-β-D-吡喃葡萄糖醛酸丁酯（3）。其中化合物3为新化合物。     

Box-Behnken效应面法优化亳菊中4种黄酮类成分提取工艺

摘要：目的:采用Box-Behnken效应面法,优选亳菊中黄酮类成分提取工艺条件。方法:在单因素试验的基础上,采用三因素三水平Box-Behnken试验设计对亳菊中黄酮类成分提取工艺参数进行优选。以乙醇浓度、料液比、提取时间为自变量,以金合欢素、木犀草素、金合欢素-7-O-β-D-葡萄糖苷及木犀草素-7-O-β-D-葡萄糖醛酸苷含量为因变量,采用Hassan方法计算总评"归一值",建立总评归一值与自变量之间的数学关系,经效应面法预测最佳工艺条件。结果:最佳提取工艺为乙醇浓度72%、料液比1:26、提取时间152min,提取三次;金合欢素、木犀草素、金合欢素-7-O-β-D-葡萄糖苷及木犀草素-7-O-β-D-葡萄糖醛酸苷含量分别为1.819 0,0.155 0,0.532 0,0.624 0mg·g-1。结论:实测值与预测值接近,表明采用Box-Behnken响应面法优化后得到的综合提取工艺参数可用于亳菊中黄酮类成分金合欢素、木犀草素、金合欢素-7-O-β-D-葡萄糖苷及木犀草素-7-O-β-D-葡萄糖醛酸苷的提取。     

高效液相色谱法同时测定维药香青兰有效部位中10个化学成分的含量

目的 建立高效液相色谱(HPLC)法同时测定维药香青兰有效部位中10个成分含量。方法 采用Shim-pack ODS(4.6 mm×250 mm, 5μm)色谱柱,流动相为乙腈(A)-0.5%甲酸溶液(B),梯度洗脱(0—30 min, 17%A;30—60 min, 17%→28%A;60—78 min, 28%A),流速为1.0 mL·min^-1;检测波长为330 nm,柱温为35℃。结果 咖啡酸、4-香豆酸、木犀草苷、木犀草素-7-O-β-D-葡萄糖醛酸苷、芹菜素-7-O-葡萄糖醛酸苷、迷迭香酸、香叶木素-7-O-β-D-葡萄糖醛酸苷、丹酚酸A、田蓟苷、香叶木素在该色谱条件下分离度良好,在考察的浓度范围内线性关系良好(r>0.999 2)。加样回收率和相对标准偏差(RSD)分别为91.83%～106.43%和0.38%～2.22%内。结论 建立的含量测定方法准确性高、重复性好,适用于香青兰有效部位的分析与质量控制研究。     

HPLC法同时测定苦碟子注射液中4种成分的含量

目的建立同时测定苦碟子注射液中绿原酸、木犀草素-7-O-龙胆二糖苷、木犀草素-7-O-β-D-吡喃葡萄糖苷和木犀草素-7-O-β-D-吡喃葡萄糖醛酸苷含量的HPLC法。方法色谱柱为Agela Pro-mosil C18柱(250 mm×4.6 mm,5μm);流动相为乙腈(A)-体积分数为1.0%乙酸水溶液(B),梯度洗脱;流速为1.0 mL.min-1;检测波长为350 nm。结果绿原酸、木犀草素-7-O-龙胆二糖苷、木犀草素-7-O-β-D-吡喃葡萄糖苷和木犀草素-7-O-β-D-吡喃葡萄糖醛酸苷的线性关系良好,线性范围分别为0.730～5.84 mg.L-1、0.530～4.24 mg.L-1、0.990～7.92 mg.L-1和2.00～16.0 mg.L-1;平均回收率分别为98.8%、99.9%、99.6%和100.6%,RSD分别为0.8%、1.1%、1.0%和0.6%(n=5)。结论该法简便、可行,重现性好,结果准确,为苦碟子注射液质量控制提供参考依据。     

地构叶黄酮类化合物的分离鉴定

从地构叶的地上部分分离得到6个黄酮类化合物，根据其性质及波谱特征分别被鉴定为香叶木素，5，7，3‘-30H-OCH3黄酮（1），木犀草素5，7，3‘4‘-4OH黄酮（2），5，7－4‘-三羟基二氢黄酮－7－O－β－D－（4″－对香豆酰）－吡喃葡萄糖苷（3），5，7，4‘－三羟基二氢黄酮－7－O－β－D（3″，对香豆酰）－吡喃葡萄糖苷（4），穗花杉双黄酮（5），木犀草素－7－O－芸香糖苷（6），所有的化合物均为首次从地构叶得到，化合物3为新化合物，命名为地构苷。     

苦碟子中的新黄酮苷(Ⅱ)

苦碟子为菊科植物抱茎苦荬菜〔Ｉｘｅｒｉｓｓｏｎｃｈｉｆｏｌｉａ(Ｂｇｅ.)Ｈａｎｃｅ〕的当年生干燥全草,具有清热解毒、消肿止痛之功效〔1〕。其主要成分为以木犀草素、芹菜素为苷元的黄酮苷.继前报〔2〕报道了两个新黄酮苷之后,又从该植物中提取分离得到一种新的黄酮苷,命名为木犀草素7ＯβＤ吡喃葡萄糖醛酸苷乙酯(ｌｕｔｅｏｌｉｎ7ＯβＤｇｌｕｃｕｒｏｎｉｄｅｅｔｈｙｌｅｓｔｅｒ,Ⅰ),此化合物为一个未见文献报道的新化合物,结构见图1.提取分离:苦碟子全草5ｋｇ,用70%的乙醇加热回流,过滤,滤液回收乙醇,经真空干燥后,浓缩液混悬于…     

木犀草素及其葡萄糖苷的半合成

以橙皮苷为原料，经３步合成了黄酮类化合物木犀草素（１），总收率３５％。本法原料易得，工艺简单，各步收率较好。同时以１通过新化合物木犀草素－７－Ｏ－β－Ｄ－葡萄糖苷四乙酸酯，合成了木犀草素－７－β－葡萄糖苷。     

苦碟子中的新黄酮苷

苦碟子为菊科植物抱茎苦荬菜［Ｉｘｅｒｉｓｓｏｎｃｈｉｆｏｌｉａ（Ｂｇｅ．）Ｈａｎｃｅ］的当年生干燥全草．具有清热解毒、排脓之功效．利用大孔树脂、硅胶柱层析及聚酰胺柱层析从中分离得到两个新的黄酮苷类成分,其中一个命名为木犀草素７ＯβＤ吡喃葡萄...     

Antioxidative constituents fromlycopus lucidus

Three phenolic compounds, rosmarinic acid (1), methyl rosmarinate (2), ethyl rosmarinate (3), and two flavonoids, luteolin (4), luteolin-7-O-beta-D-glucuronide methyl ester (5) were isolated from the aerial part of Lycopus lucidus (Labiatae). Their structures were determined by chemical and spectral analysis. Compounds 1-5 exhibited potent antioxidative activity on the NBT superoxide scavenging assay. The IC50 values for compounds 1-5 were 2.59, 1.42, 0.78, 2.83, and 3.05 microg/mL respectively. In addition, five compounds were isolated from this plant for the first time.     

中药半枝莲黄酮类成分的分离与结构鉴定

目的对中药半枝莲(Scutellaria barbata D.Don)全草的化学成分进行研究。方法应用大孔树脂、正相硅胶、反相ODS、Sephadex LH-20以及制备型高效液相等色谱法对中药半枝莲的化学成分进行了分离;并通过理化性质和光谱数据对化合物的结构进行了鉴定。结果分离鉴定了7个黄酮类化合物,分别为芹菜素(apigenin1,)、木犀草素(luteolin,2)、5,7,4'-三羟基-8-甲氧基黄酮(5,7,4'-trihydroxy-8-methoxyflvone,3)、芹菜素-7-O-β-D-葡萄糖醛酸苷(apigenin-7-O-β-D-glucuronide,4)、芹菜素-7-O-β-D-葡萄糖醛酸甲酯(apigenin-7-O-β-D-glucuronide methyl ester,5)、芹菜素-7-O-β-D-葡萄糖苷(apigenin-5-O-β-D-glucopyranoside,6)、山奈酚-3-O-β-D-芦丁糖苷(kaempferol-3-O-β-D-rutino-side,7)。结论化合物4-7为半枝莲植物中首次分离得到。     

Anti-influenza virus activities of flavonoids from the medicinal plant Elsholtzia rugulosa

ELSHOLTZIA RUGULOSA (Lamiaceae), a common Chinese herb, is widely used in the treatment of cold and fever. In order to elucidate the action mechanism and the active principles from the plant against anti-influenza virus, the influenza virus neuraminidase (NA) activity assay and IN VITRO antiviral activity assay were established, and the isolation of the active principles was guided by NA activity. Finally, 5 active constituents were obtained, namely apigenin ( 1), luteolin ( 2), apiin ( 3), galuteolin ( 4) and luteolin 3'-glucuronyl acid methyl ester ( 5), respectively. They all belong to the flavonoids. The IN VITRO antiviral assay using a cytopathic effect (CPE) reduction method showed that they all possessed anti-influenza virus activity. Among them, apigenin and luteolin exhibited the highest activities against influenza virus (H3N2) with IC (50) values of 1.43 microg/mL and 2.06 microg/mL, respectively. The structure-activity relationship (SAR) of these flavonoids with different chemical structures and their anti-influenza virus activities was addressed in this study.     

Depsides from the petals of Papaver rhoeas

Two new depsides as well as the known p-hydroxybenzoic acid and its methyl ester, protocatechuic acid, 2-(4-hydroxyphenyl)-ethanol, 2-(3,4-dihydroxyphenyl)-ethanol and the flavonoids kaempferol, quercetin, luteolin and hypolaetin and the glycosides 3- O-beta- D-glucopyranosylquercetin (isoquercitrine), 3- O-beta- D-glucopyranosylkaempferol (astragaline), 3- O-beta- D-galactopyranosylquercetin (hyperoside) were isolated from the methanol extract of the petals of Papaver rhoeas L. (Papaveraceae). The elucidation of their structures was based on NMR spectral evidence.     

刺果甘草化学成分的研究

刺果甘草(Glycyrrhiza pallidiflora Maxim)根及根茎的甲醇提取物经盐酸甲醇反应,柱层析分离,得到五个单体。经理化常数和光谱分析,确定化合物Ⅰ为β-谷甾醇,Ⅲ为macedonic acid methylester,Ⅳ为21-dehydro-macedonic acid methyl ester,命名为刺果酸甲酯(pallidifloric acid methyl ester),Ⅴ为5-羟基-4-甲氧基异黄酮,命名为刺果甘草素(pallidiflorin)。化合物Ⅱ初步确定为具有11,13(18)异环双烯的五环三萜衍生物。其中Ⅳ是首次从植物中分得,Ⅴ为新化合物。     

Influence of biotransformation of luteolin, luteolin 7-O-glucoside, 3',4'-dihydroxyflavone and apigenin by cultured rat hepatocytes on antioxidative capacity and inhibition of EGF receptor tyrosine kinase activity

Flavonoids are known as biologically active compounds. Although this has been shown by several in vivo studies, it is still elusive whether their metabolites exert similar activities. Herein we investigated the biotransformation of four different flavonoids, 3',4'-dihydroxyflavone, apigenin, luteolin and luteolin 7-O-glucoside, by cultured rat hepatocytes using a combination of enzymatic deconjugation, HPLC separation and high-resolution mass spectrometry. These flavonoids were chosen because they are active components of many plants, e. g., artichokes. All flavonoids showed rather complex metabolite patterns dominated by phase II metabolites, mainly sulfates, methyl sulfates and methyl glucuronides, but also of combined glucuronide and sulfate conjugates. Phase I metabolism by hydroxylation was rendered likely only for apigenin to form luteolin. When culture media containing the flavonoids and their metabolites were assayed for antioxidative capacity by the DPPH assay, only compounds with hydroxy groups in position 3' and 4' of the B ring were active. Thus, during metabolism of (inactive) apigenin a strong increase in the antioxidative effect was observed while that of the other three flavonoids decreased with time. Determination of EGF receptor tyrosine kinase activity likewise revealed strong inhibition in the presence of a catechol group at ring B. However, in this case the situation was much more complex resulting in a significant increase of the inhibitory activity of 3',4'-dihydroxyflavone and apigenin, but not of luteolin and luteolin 7-O-glucoside during 22 h of incubation. These results show that the biotransformation of flavonoids is very complex and may result not only in a loss but also in a gain of biological activity depending on the individual structural features.     

Adlumiceine methyl ester,a new alkaloid from Fumaria vaillantii

A new alkaloid, adlumiceine methyl ester (1), together with two known alkaloids, parfumine (2) and N-methylhydrastine methyl ester (3), was isolated from aerial parts of Fumaria vaillantii. The structures of compounds were determined by 1D/2D NMR and MS data. All three compounds were tested for cytotoxic activity against PC3 and MCF7 cell lines using Alamar blue assay. The tested compounds showed no significant cytotoxic activity (IC₅₀>50 μM) against PC3 and MCF7 cell lines.     

双(S)-萘普生甲酯的合成

目的设计合成双(S)-萘普生甲酯。方法以(S)-萘普生为原料,与溴氯甲烷反应制得的(S)-萘普生氯甲酯,然后与萘普生钾盐反应得目标化合物。结果化合物结构经1H-NMR确证。合成的双(S)-萘普生甲酯是右旋体。对其代谢过程作了初步探讨。结论合成的双(S)-萘普生甲酯是手性化合物。合成反应条件温和,产物纯度高,收率达87%。