基于化学模式识别的黄丝郁金醋炙前后HPLC指纹图谱研究

目的:建立黄丝郁金、醋黄丝郁金HPLC指纹图谱,并结合化学计量学探讨黄丝郁金醋炙前后化学成分的差异及潜在质量差异标志物。方法:收集15批四川产黄丝郁金药材并制备醋炙品,建立指纹图谱,进行相似度评价,采用SIMCA-P 14.1软件进行聚类分析、主成分分析、正交偏最小二乘判别分析。结果:建立了黄丝郁金、醋黄丝郁金指纹图谱,均确定了20个共有峰,并指认出2号峰为Bisacurone、3号峰为Bisacurone B、6号峰为双去甲氧基姜黄素、7号峰为去甲氧基姜黄素、8号峰为姜黄素、9号峰为莪术二酮、14号峰为芳姜黄酮、15号峰为吉马酮。相似度均≥0.939。聚类分析和主成分分析可基本上区分黄丝郁金、醋黄丝郁金,正交偏最小二乘判别分析共筛选出黄丝郁金醋炙前后7个质量差异标志物。结论:该研究建立的黄丝郁金、醋黄丝郁金HPLC指纹图谱结合化学计量学方法可用于探索黄丝郁金醋炙前后潜在质量标志物。

Simultaneous determination of three curcuminoids in Curcuma longa L.by high performance liquid chromatography coupled with electrochemical detection

A novel method for analysis of three active components curcumin, demethoxycurcumin and bisdemethoxycurcumin in Curcuma longa L. was developed by HPLC coupled with electrochemical detection. Three curcuminoids were well separated on a C18 column and detected with high sensitivity. A mobile phase containing acetonitrile and 10 mM Na2HPO4-H3PO4 （pH 5.0） （50：50, v/v） was used. Good linearity was obtained in the range of 0.208-41.6, 0.197-39.4, and 0.227-114μM for curcumin, demethoxycurcumin and bisdemethoxycurcumin respectively. The limit of detection reached up to 10 ？ 8 M, which was lower than that by UV detection. The relative standard deviations （RSDs） ranged from 1.06%to 1.88%for intra-day precision and from 4.30%to 5.79%for inter-day precision, respectively. The proposed method has been applied in real herb sample and recoveries ranging from 86.3%to 111%were obtained.

Use of Support Vector Regression Based on Mean Impact Value Model to Identify Active Compounds in a Combination of Curcuma longa L.and Glycyrrhiza extracts

A support vector regression based on the mean impact value (MIV) model was constructed to identify the bioactive compounds inhibiting proliferation of He La cells in a combination of turmeric (Curcuma longa L.)and liquorice (Glycyrrhiza) extracts.The quantitative chemical fingerprint from 50 batches of turmeric and liquorice extracts was established using high performance liquid chromatography hyphenated to an ultraviolet visible detector.Qualitative results were obtained using ultra performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry.A total of 46 peaks (peaks 1–15 from turmeric and 16–46 from liquorice) were selected as "common peaks" for analysis.The inhibitory effect of the combined extracts on He La cells was measured by MTT (3- (4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) assay.It was found that 15 compounds (peaks:8,12,30,24,46,11,14,9,3,1,44,18,7,45 and 43)possessing high absolute MIV exhibited a significant correlation with the cytotoxicity against He La cells; most of these have already been confirmed with potential cytotoxicity in previous research.The important potential application of the present model can be extended to help discover active compounds from complex herbal medicine prior to traditional bioassay-guided separation.It is considered that this could be a useful tool for redeveloping herbal medicine based on the use of these active compounds.

The Acute and Chronic Effects of Co-Administration of Turmeric and Black Pepper Extracts in Genetic Hypertension

High blood pressure is the main risk factor for cardiovascular diseases, it affects many people worldwide and is a public health problem. This study explored the acute and chronic actions of a mixture of turmeric (95% curcumin) plus black pepper (95% piperine) extracts, in the blood pressure pattern in spontaneously hypertensive rats (SHR) along they age. For the acute study male adult (4 - 7 months old) SHR and their control Wistar Kyoto rats (WKY) were used. A single oral dose of the mixture of turmeric/black pepper extracts (200 mg/2mg, respectively) suspension was administered. Tail-cuff was used to determine blood pressure during 180 min. For the chronic study, young (1-month-old) male SHR and their control WKY rats were fed with standard chow, or standard chow combined with cocoa, or combined with cocoa plus the mixture of turmeric/black pepper extracts;tail-cuff was used to determine blood pressure once a week, along 12 weeks. In a second chronic assay adult (5 months old) male SHR and their control WKY rats were fed with standard chow, or standard chow combined with cocoa, or combined with cocoa plus the mixture of turmeric/black pepper extracts;tail-cuff was used to determine blood pressure once a week, along 12 weeks. In all three studies, a decrease in systolic, diastolic and mean blood pressure was observed, being higher in SHR and negligible in WKY rats. The mixture of turmeric/black pepper extracts showed antihypertensive actions in SHR rats with no effect on WKY rats. The mixture delayed the onset of hypertension in young SHR rats.

姜黄标准汤剂HPLC指纹图谱结合化学模式识别研究

为了建立姜黄标准汤剂的HPLC指纹图谱,以来自四川、云南和广西的15个批次姜黄饮片为原料制备姜黄标准汤剂冻干粉,通过优化样品提取工艺和色谱条件,对姜黄标准汤剂的主要成分进行HPLC分析和化学模式识别分析。结果表明:15批姜黄标准汤剂的HPLC指纹图谱共标定了13个共有峰,确认了11、12和13号峰分别为双去甲氧基姜黄素、去甲氧基姜黄素和姜黄素;通过主成分分析筛选出了2个差异性成分(3号峰和4号峰),但目前还不能确定其所代表的物质;15批姜黄标准汤剂的相似度评价结果均大于0.9,整体可以聚为2大类,其中S5、S11和S14聚为一类,其余批次聚为一类。该HPLC指纹图谱方法呈现良好的精密度、重复性和稳定性,可为姜黄标准汤剂及中药配方颗粒产品质量控制提供参考和帮助。

HPLC-ESI-MS/MS分析姜黄中姜黄素类化合物

运用HPLC-ESI-MS/MS方法分析姜黄中姜黄素类化合物。利用高效液相色谱-电喷雾多级串联质谱(HPLC-ESI-MSn)技术,以Venusil XBP C18(2.1×150 mm,5μm,Agela Technologies)作为分离色谱柱,乙腈和水为流动相,电喷雾离子源(ESI),正负离子同时扫描。根据谱峰的保留时间和质谱一、二级离子碎片信息,结合对照品及参考文献信息,同时检测出姜黄中28种姜黄素类化合物,其中有8种化合物尚未见从姜黄中报道,并解析了它们的二级质谱断裂规律。本文为更加全面研究姜黄中姜黄素类化合物提供参考。

HPLC法测定姜黄、郁金、广西莪术中姜黄素的含量

目的 测定不同产地姜黄、郁金、广西莪术中姜黄素的含量。方法 采用超声提取法 ,色谱柱 Supelcosil TML C1 8柱 (5μm ,4 .6 m m× 2 5 0 mm ) ,流动相为甲醇 -异丙醇 - 0 .5 %醋酸溶液 (19∶ 2 5∶ 5 6 ) ,流速 0 .6 m L /m in,测定波长 4 2 0 nm,柱温 35℃。结果 姜黄素在 14～ 5 6 μg范围内线性关系良好 (r=0 .9995 ) ,平均回收率 99.82 % ,RSD为 1.5 7%。结论 本法准确、快速 ,为控制中药原料药姜黄、郁金。

不同干燥方式对姜黄中姜黄素和姜黄油的影响

以新鲜姜黄根茎为原料,采用高效液相色谱法、水蒸气蒸馏法及气相色谱质谱联用(GC-MS)等方法研究了晒干、阴干、30℃热风烘干、60℃热风烘干和冷冻干燥5种干燥方式对姜黄素的相对含量和姜黄油组分组成的影响。结果表明,不同干燥方式下,姜黄素的相对含量和姜黄油的含量及组分的变化较大,但姜黄的色度变化较小,其中自然阴干方式下姜黄素和姜黄挥发油含量相对较高,分别为1.84%、6.15%。研究结果为姜黄的开发利用和产品加工提供一定的技术支持。

缅甸进口姜黄无机元素分析研究

通过测定缅甸进口姜黄中26种无机元素,并对进口姜黄中重金属含量进行风险评价,为缅甸进口姜黄的质量控制奠定基础。采用微波消解-电感耦合等离子体质谱(ICP-MS)法对24批来自缅甸地区的姜黄中的26种无机元素进行测定,通过靶标危害系数(THQ)和总危害指数(HI)对Pb、Cd、Cu 3种元素进行非致癌风险评价,用终生致癌风险(R)对As进行致癌风险评价。结果表明,缅甸进口姜黄中含有24种无机元素,其中K、Na、Mg、Ca 4种营养元素含量占24种无机元素的92.39%。缅甸姜黄中均未检出Sn、Hg 2种金属元素,Pb、Cd、As、Cu、Hg 5种重金属元素含量均符合2020版《中国药典》限定值。经过缅甸姜黄中Cu、Pb、Cd 3种重金属元素健康风险评价,THQ和HI均小于1,表明人体通过缅甸姜黄摄入的Cu、Pb、Cd不会对人体造成非致癌伤害。经过对姜黄中As的致癌健康风险评价,致癌风险R为7.72×10-6,低于世界卫生组织建议的致癌风险值(1.00×10-5),通过缅甸姜黄摄入的总As不存在致癌风险。总体而言,缅甸进口姜黄重金属元素保持在较好水平。

固相萃取-HPLC法测定生姜不同品种和器官中姜黄素含量(英文)

用固定萃取-HPLC法研究了生姜不同品种、同一品种不同产地及不同器官中姜黄素含量。生姜干粉用4倍量75%乙醇提取2次,提取液过C18固相萃取柱,80%的乙醇洗脱,HPLC测定姜黄素含量。13个不同品种或产地的生姜中,山东、潮州和湖北产的山东大肉姜姜黄素含量分别为0.76、1.11和0.75mg/100g干重,广西白肉姜、云南黄姜、潮州南姜、安徽菜姜、四川姜、四川小黄姜、梅县水姜、清远火姜、广州疏轮大肉姜和有机栽培的广州大肉姜的姜黄素含量分别为1.5450、1.08、0.84、0.92、1.16、1.00、2.63、2.86、2.20和5.01mg/100g干重。有机栽培的广州大肉姜的姜肉、姜皮和地上部茎叶中姜黄素含量分别为4.49、1.2和0.41mg/100g干重。但生姜中姜黄素含量远低于贵州产姜黄的含量(2857mg/100g干重)。结果表明,生姜中姜黄素含量主要取决于品种,栽培地理位置对其有较少的影响。有机栽培可大大提高姜黄素含量。

HPLC法测定姜黄提取物中有效成分含量

目的：建立高效液相色谱法同时测定姜黄提取物中姜黄素、一脱甲氧基姜黄素、二脱甲氧基姜黄素的含量.方法：采用C18色谱柱（150 mm×6 mm,5μm）,流动相为乙腈-水-冰乙酸（39∶57∶4）,流速为1.4 ml· min-1;检测波长：428 nm;柱温：35℃;进样量：20μl.结果：同时测定了姜黄素、一脱甲氧基姜黄素、二脱甲氧基姜黄素的含量,三者的线性范围分别为81.31～650.50 μg ·ml-1,26.93 ～215.42μg· ml-1,16.32～130.54 μg ·ml-1.平均回收率分别为100.9％,100.9％,100.6％,RSD分别为1.7％,1.2％,1.5％（n=9）.结论：该方法简便、准确、重复性好,可用于姜黄提取物中有效成分的测定.

基于姜黄中姜黄素类成分与姜黄粉末颜色指数L＊、a＊、b＊值的相关性分析

目的：初步探究姜黄中姜黄素类成分含量与测色仪所得姜黄药材粉末颜色指数L＊、a＊、b＊间的关系,为姜黄药材质量评价提供科学依据。方法：运用中国药典方法检测姜黄中姜黄素、去甲氧基姜黄素、双去甲氧基姜黄素的含量,并求得总姜黄素含量。测色仪测得姜黄粉末的颜色指数L＊、a＊、b＊。最后用灰色关联度法、Pearson相关系数以及回归分析探求含量与颜色间的联系。结果：通过3种统计学分析法可知,姜黄素类成分含量与a＊值间确实存在一定的相关性,且呈正相关性,而b＊值、L＊值与姜黄成分的关系尚不明确。结论：姜黄素类成分的含量与药材粉末颜色红的程度关系密切,即含量越高,粉末颜色越红。颜色指数a＊的大小可作为判别姜黄药材质量优劣的重要依据。

HPLC法测定姜黄中姜黄素类化合物的含量

采用高效液相色谱法测定姜黄中主要姜黄素类化合物,色谱柱为C18,流动相为乙腈和0.5%冰醋酸,采样梯度洗脱,检测波长为425 nm。结果表明,姜黄样品中姜黄素类化合物的加样回收率分别为99.87%,99.91%,99.51%,RSD分别为0.75%,1.217%,1.06%。本方法对测定姜黄中主要的姜黄素类化合物快速简单,重复性好,为植物提取行业的含量测定提供依据。

饲用植物姜黄粗提物HPLC特征图谱的建立

研究建立饲用植物姜黄粗提物的高效液相色谱(HPLC)特征图谱。采用Sunfire C18(4.6 mm×250 mm,5μm,Waters)色谱柱,以乙腈和0.1%甲酸水为流动相进行梯度洗脱,流速1.0 mL/min、柱温35℃、检测波长254 nm、进样量10μL。成功建立30批姜黄粗提物的HPLC特征图谱,确定8个特征峰,指认3个色谱峰,分别为双去甲氧基姜黄素、去甲氧基姜黄素、姜黄素。试验表明,该方法具有良好的精密度、重复性、稳定性。

HPLC法测定姜黄中去甲氧基姜黄素的含量

目的:测定姜黄中去甲氧基姜黄素的含量。方法:采用超声波提取法和柱层析法,Prep Nova-Pak HR C_(18)柱(5μm,250mm×4.6mmI.D),流动相为乙腈:水=41:53+10%冰醋酸;检测波长为254nm;流速为1.2ml/min;柱温为35℃。结果:去甲氧基姜黄素在9～150μg/ml浓度范围内线性关系良好(r=0.9998),回收率97.24%,RSD为2.0%。结论:方法准确、快速,为测定姜黄中去甲氧基姜黄素的含量提供了依据。

Identification of Extracts Responsible for the Effect of Tick Reppeling Activity of Turmeric

Turmeric (Curcuma longa L.) is one of the essential condiments all over the world. Turmeric is an important medicine in the eastern medical systems and its therapeutic properties have been well recorded. Curcumin, commonly called diferuloyl methane (hydrophobic polyphenol), was studied extensively for its biological properties. Sri Lankan turmeric records relatively higher percentage (up to 9%) of curcumin. The bioactive compounds with insecticidal or pesticidal activity were studied from the Sri Lankan turmeric as there is an increasing demand for natural products to control ticks and fleas in dogs against the chemicals that induce some secondary effects. Fifty grams (50 g) of dried coarsely ground turmeric (Curcuma longa L.) was subjected to sequential extractions with four different solvents in ascending order of polarity using Soxhlet apparatus. The treatments consisted of solvent-fractionated turmeric extracts from hexane, dichloromethane (CH2Cl2), ethyl acetate (EtOAc) and Methanol (CH3OH) dissolved in the water to 100 ppm. The test carried out using a modified olfactometer and the degree of repellency of common tick species Rhipicephalus sanguineus was recorded. The hexane extract from dried turmeric powder showed the highest repellence of 80% whereas other fractions showed lesser repellence. Further studies in the direction of purification, dose dependent repellency and persistency.

姜黄种质资源地下部性状遗传多样性分析与综合评价

为筛选姜黄优良育种材料,本研究对72份姜黄种质资源地下部的农艺性状、指标性成分、颜色值等指标进行遗传多样性分析、主成分分析以及聚类分析。结果表明,各指标性状变异范围在0.11~1.19之间,姜黄资源类型较丰富;姜黄资源遗传多样性指数为5.32~6.16。相关性分析结果表明,姜黄地下部的农艺性状、指标性成分、颜色值间存在显著相关性。主成分分析将21个指标转换为6个综合因子,累积贡献率为81.351%。聚类分析将姜黄种质资源分为3个类群,各类群在产量、姜黄素类成分含量、挥发油含量、母姜性状间有明显的区别,从产量、质量2个方面考虑,筛选出15份优异姜黄种质资源。

姜黄总多酚大孔树脂纯化工艺研究

目的:比较6种不同极性大孔树脂对姜黄多酚的吸附性能,并确立纯化工艺参数。方法:采用福林酚显色法测定多酚含量;采用静态吸附、解吸附实验对6种大孔树脂进行筛选,确定最佳树脂;依据吸附和解吸附条件进行单因素实验,确定最佳工艺条件。结果:AB-8型大孔树脂的吸附-解吸性能最佳;纯化姜黄多酚的最佳静态吸附条件为:吸附时间7 h,样液浓度15 mg/mL,样液pH=4;最佳静态解吸条件为:解吸附时间2 h,乙醇浓度80%,pH=8;最佳动态吸附条件为:径高比1∶4,样液浓度25 mg/mL,样液pH=5,上样流速1.5 mL/min;最佳动态解吸条件为:乙醇浓度80%,乙醇pH=8,洗脱流速1.5 mL/min。结论:此工艺条件操作简单,经济成本低,为姜黄的进一步开发利用提供了参考依据。

真空膜蒸馏处理中药姜黄清洗废水工艺研究

探究了真空膜蒸馏过程工艺对中药姜黄清洗废水处理性能的影响,评价了最优工艺条件下真空膜蒸馏对清洗废水的连续处理效果.结果表明,在进料温度为65℃、进料流量750 mL/min、渗透侧真空度0.09 MPa的条件下,膜通量最高可达到51.35 kg/(m^(2)h).连续运行8 h后,渗透液中COD质量浓度低至21.14 mg/L,氨氮、总氮、总磷质量浓度均小于0.5 mg/L,水质完全满足《中药类制药工业水污染物排放标准(GB 21096-2008)》中所规定的排放限值,同时达到了《城市污水再生利用工业用水水质(GB/T 19923-2005)》中所规定的再生水回用标准.

Three new sesquiterpenes from roots of Curcuma longa

Objective:To study the chemical constituents from the roots of Curcuma longa.Methods:The structures of the compounds were elucidated based on extensive spectral analysis,including 1D and 2D NMR,MS,UV,and CD analysis.Results:Two new sesquiterpene compounds(1S,2R,5R,7S,8R)-2,8-epoxy-5-hydroxybisabola-3,10-dioen-9-one(1),(1R,2R,5R,7S,8R)-2,8-epoxy-5-hydroxybisabola-3,10-dioen-9-one(2),and a new natural product 6-(4-Hydroxymethylphenyl)-2-methyl-hept-2-ene-4-one(3)together with three known compounds ar-turmerone(4),2-methyl-6-(4-hydroxyphenyl-3-methyl)-2-hepten-4-one(5)and 2-methyl-6-(4-hydroxyphenyl)-2-hepten-4-one(6)were isolated from C.longa root extract with 95%ethanol.Conclusion:In the study,three new compounds were isolated from C.longa,and their absolute configurations were determined.