RP-HPLC法测定中药木贼中黄酮醇苷的含量

目的建立以高效液相法测定中药木贼中一个黄酮醇苷山奈酚-3-双葡萄糖苷的含量方法。方法色谱柱为Calesil ODS-100(250 mm×4.6 mm,5μm),流动相为甲醇-水(45:55),流速为1.0 ml/min,检测波长254 nm,柱温30℃,进样量10μl。结果山奈酚-3,7-双葡萄糖苷的检测浓度在0.003 12~0.104 mg/ml范围内与峰积分面积呈良好线性关系(r=0.999 9),平均回收率为100.2%,RSD=1.74%(n=9)。3个不同产地批号的样品中山奈酚-3-双葡萄糖苷的含量均在0.30%以上。结论该方法简便、快捷、重复性好,可作为木贼药材的质量控制的方法。     

基于多成分定量分析结合薄层色谱检查的颠茄流浸膏质量评价

目的建立颠茄流浸膏中同时测定4种指标成分含量的方法,结合薄层色谱检查,为其质量评价提供依据。方法采用HPLC,色谱柱:Agilent Kromesil 100-5 C18柱(4.6 mm×250 mm,5μm),流动相为甲醇-0.05%甲酸溶液,梯度洗脱,流速1.0 mL·min^-1,柱温为30℃。采用薄层色谱法进行阿托品检查。结果 4种活性成分东莨菪苷在0.065 76~0.657 6μg(r=1.000 0)、山柰酚-3-O-半乳糖-(6→1)鼠李糖-7-O-葡萄糖苷在0.082 16~0.821 6μg(r=0.999 9)、东莨菪内酯在0.049 84~0.498 4μg(r=1.000 0)和芦丁在0.010 00~0.099 98μg(r=0.999 9)内,均呈良好线性关系;东莨菪苷、山柰酚-3-O-半乳糖-(6→1)鼠李糖-7-O-葡萄糖苷、东莨菪内酯和芦丁的加样回收率分别为100.6%,99.8%,99.9%和97.9%,RSD分别为1.4%,1.6%,1.4%和1.5%。部分批次指标成分含量低且检出硫酸阿托品。结论建立的含量测定方法灵敏度高,结果准确,适用于颠茄流浸膏的质量评价。     

HPLC法同时测定三叶青块根中6个黄酮类成分的含量

目的:建立同时测定三叶青块根中芦丁、异槲皮苷、山柰酚-3-O-芸香糖苷、紫云英苷、槲皮素和山柰酚含量的方法。方法:采用高效液相色谱(HPLC)法。色谱柱为Alliance SilGreen C18,流动相为0.2%磷酸水溶液-乙腈溶液(梯度洗脱),流速为1.0mL/min,柱温为35℃,检测波长为360 nm,进样量为15μL。结果:芦丁、异槲皮苷、山柰酚-3-O-芸香糖苷、紫云英苷、槲皮素和山柰酚的检测质量浓度线性范围分别为21.77～217.77、12.37～123.75、13.23～132.31、4.63～46.30、5.75～57.50、3.36～33.66μg/mL(r均=0.999 9);检测限分别为0.217 8、0.123 8、0.066 2、0.046 3、0.191 7、0.112 3μg/mL;定量限分别为0.435 6、0.247 5、0.165 4、0.154 3、0.575 0、0.421 2μg/mL;精密度(n=6)、稳定性(24 h,n=7)、重复性(n=6)试验的RSD均≤3.20%;平均加样回收率分别为96.23%、86.88%、97.51%、97.67%、97.50%、87.46%,RSD分别为1.85%、1.90%、1.84%、1.87%、1.25%、2.01%(n=9)。结论:该方法快速、简便,可用于同时测定三叶青块根中芦丁、异槲皮苷、山柰酚-3-O-芸香糖苷、紫云英苷、槲皮素和山柰酚的含量。     

HPLC法同时测定不同产地蔓性千斤拔中5个异黄酮成分的含量北大核心CSCD

目的:建立同时测定不同产地蔓性千斤拔药材中染料木素-4′,7-二-O-葡萄糖苷、大豆苷元-7-O-β-D-葡萄糖苷、染料木素-6-C-葡萄糖苷、5,4’-二羟基异黄酮-7-O-β-D-吡喃木糖基-(1→6)-β-D-吡喃葡萄糖苷、染料木苷5个异黄酮类化合物含量的高效液相色谱法。方法:采用Diamonsil C_(18)色谱柱(250 mm×4.6 mm,5μm),以乙腈(A)-0.2%磷酸水溶液(B)为流动相,梯度洗脱,流速1.0 mL·min^(-1),检测波长258 nm,柱温30℃。结果:染料木素4′,7-二-O-葡萄糖苷、大豆苷元-7-O-β-D-葡萄糖苷、染料木素-6-C-葡萄糖苷、5,4’-二羟基异黄酮-7-O-β-D-吡喃木糖基-(1→6)-β-D-吡喃葡萄糖苷和染料木苷进样量分别在0.033~0.656μg(r=0.999 7)、0.010~0.204μg(r=0.999 5)、0.034~0.687μg(r=0.999 9)、0.012~0.244μg(r=0.999 7)和0.086~1.725μg(r=0.999 9)范围内与峰面积呈现良好的线性关系;平均回收率(n=6)分别为98.11%、94.27%、93.17%、93.13%和98.97%,RSD分别为1.0%、1.6%、1.4%、1.4%和1.8%。测得染料木素4′,7-二-O-葡萄糖苷、大豆苷元-7-O-β-D-葡萄糖苷、染料木素-6-C-葡萄糖苷、5,4’-二羟基异黄酮-7-O-β-D-吡喃木糖基-(1→6)-β-D-吡喃葡萄糖苷和染料木苷的样品含量分别为0.112~0.192、0.047~0.072、0.110~0.170、0.074~0.115和0.437~0.703 mg·g^(-1)。结论:经方法学验证,本法可用于蔓性千斤拔药材的质量控制。     

侧柏叶炮制前后成分的对比

目的建立HPLC法测定侧柏叶及其炮制品中杨梅苷、槲皮苷、杨梅素、槲皮素、山柰酚、穗花杉双黄酮及扁柏双黄酮的含量,对比侧柏叶炮制前后7种成分的含量变化。方法采用药典法进行炮制。色谱柱为Welch Ultimate LP-C18(4.6 mm×250 mm,5μm),流动相为甲醇-0.2%磷酸水梯度洗脱,检测波长为330 nm,流速1 m L/min。结果杨梅苷、槲皮苷、杨梅素、槲皮素、山柰酚、穗花杉双黄酮及扁柏双黄酮的标准曲线呈良好的线性关系(r≥0.999 5),各组分平均回收率在97.6%~101.1%之间,RSD≤1.14%(n=6)。炮制后,杨梅苷、槲皮苷、穗花杉双黄酮及扁柏双黄酮含量降低,而杨梅素、槲皮素及山柰酚含量相对升高。结论所建立的HPLC法简便易行,可用于侧柏叶、侧柏炭的含量测定。侧柏叶炮制前后成分种类和量的改变,表明其炮制过程存在着成分转化过程。     

毛菊苣中山柰酚-3-O-β-D-葡萄糖醛酸苷和山柰酚-3-O-β-D-吡喃葡萄糖苷对照品的制备研究

目的建立维药毛菊苣中山柰酚-3-O-β-D-葡萄糖醛酸苷和山柰酚-3-O-β-D-吡喃葡萄糖苷对照品的制备分离方法。方法取毛菊苣药材醇提浸膏的乙酸乙酯萃取部位上样于硅胶柱色谱分离,收集黄酮苷富集流份,继续用凝胶柱色谱及制备HPLC进行分离纯化,通过NMR、MS等波谱方法鉴定化合物结构,经TLC、HPLC-UV及MS联用等技术进行质量分数检测。结果制备分离得到2个化合物分别鉴定为山柰酚-3-O-β-D-葡萄糖醛酸苷(1)和山柰酚-3-O-β-D-吡喃葡萄糖苷(2),质量分数均大于98%,其中2为首次从该属植物中分离得到。结论该法制备得到的2个黄酮苷类对照品符合中药化学对照品的相关技术要求,为药材毛菊苣和含毛菊苣的成方制剂的质量控制及药效物质基础研究提供化学对照品。     

HPLC法同时测定覆盆子中7个成分的含量

摘要：目的:建立同时测定覆盆子中鞣花酸、山柰酚-3-O-芸香糖苷、椴树苷、山柰酚、槲皮素、芦丁和齐墩果酸含量的方法。方法:采用HPLC色谱法,色谱柱为Thermo ODS C18（250 mm×4.6 mm,5μm）,以乙腈-0.2%磷酸水溶液为流动相,梯度洗脱,流速:1.0 ml·min-1,检测波长:254 nm（鞣花酸、槲皮素、山柰酚）、340 nm（山柰酚-3-O-芸香糖苷、芦丁）、360 nm （齐墩果酸）、316 nm（椴树苷）,柱温:30℃,进样量:20μl。结果:鞣花酸、山柰酚-3-O-芸香糖苷、椴树苷、山柰酚、槲皮素、芦丁和齐墩果酸检测质量浓度的线性范围分别为14.412～172.944μg·ml-1,5.042～60.504μg·ml-1,0.605～7.260μg·ml-1,1.151～13.812μg·ml-1,2.562～30.744μg·ml-1,4.451～53.412μg·ml-1,0.507～6.084μg·ml-1（r为0.999 4～0.999 9）;平均加样回收率分别为101.3%,99.6%,100.5%,100.8%,101.0%,99.7%,100.3%（RSD<2.0%,n=6）。结论:该方法操作简便、结果准确、重复性好,可用于覆盆子的质量控制。     

HPLC双波长法研究八角莲饮片的质量

目的研究八角莲饮片的质量控制新标准。方法用HPLC双波长法同时检测八角莲饮片中鬼臼毒素、4′-去甲基鬼臼毒素、山柰酚和槲皮素。确定了360 nm作为槲皮素和山柰酚的定量波长,290 nm作为鬼臼毒素与4′-去甲基鬼臼毒素的定量波长;柱温:30℃;流速:1.0 mL·min~(-1);进样量:10μL。结果 HPLC双波长法可以同时测定八角莲饮片中的4种成分。鬼臼毒素、4′-去甲基鬼臼毒素、山柰酚和槲皮素的线性范围分别为0.74～3.68,2.40～12.02,0.21～1.08和0.26～1.28μg;回收率分别为99.56%,100.22%,100.67%和100.44%;含量分别为9.46～31.53,0.64～12.08,1.78～2.55和1.10～2.45 mg·g~(-1)。结论该方法快速、简捷、稳定可靠,适用于八角莲中木脂素类和黄酮类化学成分的测定。同时,该结果也表明各批次间黄酮类成分的差异较木脂素类成分小。     

多波长高效液相色谱法同时测定夜宁合剂中4种有效成分的含量

目的建立多波长HPLC梯度洗脱法测定夜宁合剂中(-)-丁香树脂酚-4-O-β-D-呋喃芹糖基-(1→2)-β-D-吡喃葡萄糖苷、女贞苷、特女贞苷和槲皮苷的含量。方法采用C18色谱柱(250 mm×4.6mm,5μm);流速:1.2 mL·min-1;流动相A为乙腈-甲醇(1:2),B为0.1%磷酸溶液,梯度洗脱;检测波长:(-)-丁香树脂酚-4-O-β-D-呋喃芹糖基-(1→2)-β-D-吡喃葡萄糖苷为204 nm,女贞苷和特女贞苷为224 nm,槲皮苷为360 nm,柱温为30℃。结果 (-)-丁香树脂酚-4-O-β-D-呋喃芹糖基-(1→2)-β-D-吡喃葡萄糖苷、女贞苷、特女贞苷和槲皮苷质量浓度分别在5.75¹15.00μg·mL-1(r=0.999 7)、6.45115.00μg·mL-1(r=0.999 7)、6.45¹29.00μg·mL-1(r=0.9995)、5.30129.00μg·mL-1(r=0.9995)、5.30¹06.00μg·mL-1(r=0.999 9)、8.45106.00μg·mL-1(r=0.999 9)、8.45¹69.00μg·mL-1(r=0.999 8)与峰面积线性关系良好;(-)-丁香树脂酚-4-O-β-D-呋喃芹糖基-(1→2)-β-D-吡喃葡萄糖苷、女贞苷、特女贞苷和槲皮苷的平均加样回收率分别为97.7%、96.8%、98.8%、98.2%,RSD(n=6)分别为1.5%、0.60%、1.1%、1.1%。结论该方法快速、灵敏、准确,可作为夜宁合剂的含量控制方法。     

HPLC同时测定肿节风中3种成分的含量

目的：建立HPLC法同时测定肿节风中异嗪皮啶-7-O-β-D-葡萄糖苷、异嗪皮啶和山柰酚-3-O-β-D-葡萄糖酸苷的含量。方法：色谱柱：Waters XBridge C18柱（250mm&#215;4．6mm，5μm）；流动相：0．1％醋酸甲醇溶液（A）-0．1％醋酸水溶液（B），梯度洗脱（0～17min，A：25％，B：75％；17—65min，A：25％→55％，B：75％→45％）；流速为0．5mL&#183;min^-1；检测波长为344nm；柱温26℃。结果：异嗪皮啶-7-O-β-D-葡萄糖苷、异嗪皮啶和山柰酚-3-O-β-D-葡萄糖酸苷的线性范围分别为0．2～4．0μg（r=0．9999），0．2～4．0μg（r=0．9999），0．5～10μg（r=0．9999）；平均回收率（n=5）分别为100．6％（RSD=1．7％），99．8％（RSD=1．1％），99．6％（RSD=0．4％）。结论：所建立的HPLC方法操作简便，准确可靠，分离度好，为全面评价肿节风药材的质量提供了实验依据。     

山萘酚-3-O-芸香糖苷磷脂复合物的制备与理化性质研究

目的：山萘酚-3-O-芸香糖苷磷脂复合物的制备和理化性质考察。方法：制备山萘酚-3-O-芸香糖苷的磷脂复合物,测定其与山萘酚-3-O-芸香糖苷的溶解度,并对两者的水油分配系数进行分析。结果：与山萘酚-3-O-芸香糖苷相比,磷脂复合物不仅在正辛醇中溶解性有明显改善,在水中溶解度也有所升高;在不同pH的水一正辛醇系统中,复合物的表观油一水分配系数与山萘酚-3-O-芸香糖苷相比有一定的差异。结论：山萘酚-3-O-芸香糖苷磷脂复合物可明显改善山萘-3-O-芸香糖苷在水正辛醇中的溶解性能。     

Antiulcerogenic Activity of Alhagi maurorum.

Abstract

Six main flavonoid glycosides were isolated, for the first time, from the ethanol extract of Alhagi maurorum Boiss (Leguminosae).. They were identified as kaempferol, chrysoeriol, isorhamnetin, chrysoeriol-7-O.-xylosoid, kaempferol-3-galactorhamnoside, and isorhamnetin 3-O.-β-D-apio-furanosyl (1-2) β-D-galactopyranoside. Their identities were established by m.p., UV, EI-mass, Fab-mass, 600 MHz ¹H and ¹³C NMR. The total extract (300 and 400 mg/kg) and two of the isolated compounds (chrysoeriol 7-O.-xylosoid and kaempferol-3-galactorhamnoside, 100 mg/kg each) showed a very promising antiulcerogenic activity with curative ratios 66.31%, 69.57%, 75.49%, and 77.93%, respectively.     

高效液相色谱法测定肿节风药材中异秦皮啶与山柰酚-3-O-葡萄糖醛酸苷的含量

目的建立肿节风药材中山柰酚-3O-葡萄糖醛酸苷与异秦皮啶的含量测定方法。方法色谱柱为Kromasil ODS-1（4．6mm×250mm,5μm）,流动相为乙腈-0．1％磷酸水溶液,梯度洗脱,流速为1．0mL·min^-1,检测波长为344nm,柱温为25℃。结果山柰酚-3-O-葡萄糖醛酸苷在0．2006～4．012μg线性关系良好,相关系数r=0．9999．平均回收率为100．1％,RSD=1．8％;异秦皮啶在0．4352～8．704μg线性关系良好,相关系数r=0．9999．平均回收率为99．8％,RSD=1．5％。结论所用方法简便、准确,重复性好,在同一高效液相色谱条件下可同时测定山柰酚-3-O-葡萄糖醛酸苷和异秦皮啶的含量,提供了更好的控制肿节风药材质量的方法。     

Flavonoids and aromatic compounds from the rhizomes of<Emphasis Type="Italic">Zingiber zerumbet</Emphasis>

Repeated column chromatography of the CHCl3-soluble fraction of Zingiber zerumbet led to the isolation and identification of two aromatic compounds, p-hydroxybenzaldehyde (1) and vanillin (2), and six kaempferol derivatives, kaempferol-3,4',7-O-trimethylether (3), kaempferol-3-O-methylether (4), kaempferol-3,4'-O-dimethylether (5), 4'-O-acetylafzelin (6), kaempferol-3-O-(4-O-acetyl-alpha-L-rhamnopyranoside)], 2',4'-O-diacetylafzelin (7), kaempferol-3-O-(2,4-O-diacetyl-alpha-L-rhamnopyranoside)], and 3',4'-O-diacetylafzelin (8), kaempferol-3-O-(3,4-O-diacetyl-alpha-L-rhamnopyranoside)]. The structures of 1-8 were identified by analysis of spectroscopic data as well as by comparison with published values. This is the first report on the isolation of compounds 1-3 from this plant.     

Antioxidant activities of new flavonoids from <Emphasis Type="Italic">Cudrania tricuspidata</Emphasis> root bark

Two new flavonoids, hydroxybenzyl flavonoid glycosides (6-p-hydroxybenzyl kaempferol-7-O-β-D-glucopyranoside named cudranian 1 and 6-p-hydroxybenzyl quercetin-7-O-β-D-glucopyranoside named cudranian 2), and 3 known flavonoids (kaempferol-7-O-β-D-glucopyranoside, quercetin-7-O-β-D-glucopyranoside and aromadendrin) were isolated from root bark of Cudrania tricuspidata and their structures were elucidated by spectroscopic methods. These compounds showed remarkable radical scavenging effects against 1, 1-diphenyl-2-picrylhydrazyl (DPPH) and anti-lipid peroxidation efficacy on human low-density lipoprotein by TBARS assay.     

Antioxidant Potential of Gynura procumbens

Abstract

The leaves of Gynura procumbens (Merr.) Compositae, commonly called “sambung nyawa” in Malaysia, are often eaten raw with rice. The methanol extract was prepared from the dried leaves using a Soxhlet apparatus. The methanol extract was then fractionated into chloroform, ethyl acetate, n-butanol, and aqueous fractions using a separating funnel. In the current study, the antioxidant potency of G. procumbens extract and fractions were investigated, employing various established in vitro systems, such as trolox equivalent antioxidant capacity, β -carotene–linoleic acid model system, 1,1-diphenyl-2-picrylhydrazyl (DPPH) scavenging, reducing power, and xanthine oxidase inhibitory activity. Based on the results obtained, the extract and fractions showed different antioxidant potential. Among the fractions, the ethyl acetate fraction displayed higher antioxidant properties. The contents of the potential antioxidant component of the extract and fractions were also determined using HPTLC densitometric and spectrophotometric (using Folin-Ciocalteu reagent) methods. HPTLC study revealed that the methanol extract and the ethyl acetate and n-butanol fractions contain 0.74% and 2.9%, 7.76% and 12.75%, and 4.52% and 0.33% of kaempferol-3-O-rutinoside and astragalin, respectively. The total phenolic content of the extract and fractions varied from 4.37% to 23.43% of dry weight, expressed as gallic acid equivalents (GAE). With further data analysis, it was found there was a significant correlation (p < 0.05) between the total phenolic content of the sample and its DPPH scavenging activity and reducing power with correlation coefficients (r) of 0.891 and 0.926, respectively. These results suggest that phenolics in these plants provide substantial antioxidant activity.     

Role of Blepharis maderaspatensis and Ammannia baccifera plant extracts on in vitro oxygen radical scavenging,secretion of gastric fluid and gastroprotection on ulcer induced rats

Context: Blepharis maderaspatensis L. Roth (BM) (Acanthaceae) and Ammannia baccifera L. (AB) (Lythraceae) are used in folk medicine for various stomach disorders.

Objective: The chloroform and ethanol extracts of both plants were evaluated for antioxidant, gastric antisecretory, and gastroprotective properties.

Methods: Antioxidant properties of the extracts were evaluated using 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging assay and nitric oxide (NO) scavenging assay. The gastric antisecretory properties of the extracts were assessed, at a dose of 100 and 200 mg/kg, using aspirin-pylorus ligation induced gastric ulcer models and the gastroprotective activity of the extracts was assessed, at a dose of 100 and 200 mg/kg, using HCl-ethanol induced ulcer models in rats.

Results and discussion: Ethanol extract of BM (EBM) possessed good antioxidant property with IC₅₀ values of 37.4 and 44.1 µg/mL in DPPH and NO scavenging assays respectively, where 25–250 µg/mL concentration in DPPH assay and 30–300 µg/mL concentration in NO scavenging assay were used. Ethanol extract of AB (EAB) at a dose of 200 mg/kg reduced the free acidity to 142.66 mEq/L and total acidity to 451.22 mEq/l. It reduced the gastric secretion with increase in pH from 2.2 to 3.15. Possessing good antisecretory activity, it also reduced the ulcer by 92.2% in aspirin and pylorus ligation induced gastric ulcer models. EAB increased the mucus secretion and adherent mucus in the tissues with a 71.43% reduction of ulcerin HCl-ethanol induced ulcer models, at a dose of 200 mg/kg. This activity can be attributed to the various flavonoids like rutin and kaempferol-3-O-β-glucopyranoside, and the phytosterol, β-sitosterol-3-O-β-glucopyranoside, and phenolics present in the extracts.

Conclusion: EBM possessed significant antioxidant property while EAB possessed good antisecretory and gastroprotective activity.     

A new chromone from Cassia nodosa

A new chromone named as 5,4'-dihydroxy-7-methyl 3-benzyl chromone (1) along with three known flavonoid compounds as unsubstituted flavone, kaempferol-3-o-rhamnoside and quercetin-3-o-arabinoside have been isolated from the leaves of Cassia nodosa. Their structures have been established by means of chemical and spectral evidences (IR, UV, ¹H-NMR, ¹³C-NMR and mass spectra).