高效液相色谱法同时测定槐枝中芦丁和槲皮素

提出了用高效液相色谱法同时测定槐枝中芦丁和槲皮素含量的方法。采用ZORBAXEclipse XDB-C18色谱柱(4.6 mm×250 mm,5μm)为固定相,以甲醇-0.01 mol.L-1乙酸铵(47+53)混合溶液为流动相,在360 nm波长处用二极管阵列检测器检测。芦丁和槲皮素的质量分别在0.015 4~0.154 0,0.010 8~0.108 0 mg.L-1之间与其相应的峰面积呈线性关系,检出限分别为(3S/N)分别为0.06,0.008μg.g-1。应用此法测定槐枝样品中芦丁和槲皮素的含量,加标回收率分别为97.4%~98.8%,97.4%~98.2%;相对标准偏差(n=6)分别为1.6%,1.8%。     

高效液相色谱法同时测定玫瑰花口服液中没食子酸、芦丁、槲皮素和山奈素

建立了同时测定玫瑰花口服液中没食子酸、芦丁、槲皮素和山奈素的高效液相色谱(HPLC)测定方法。采用Agilent HC-C18色谱柱(250×4.6mm,5μm);流动相为0.5%磷酸-甲醇,梯度洗脱;流速0.8mL·min-1;柱温30℃;检测波长260nm。结果显示:没食子酸在40.7～244.20μg·mL-1、芦丁在25～150μg·mL-1、槲皮素在13.3～80μg·mL-1、山奈素在2.69～16.2μg·mL-1线性关系良好,相关系数分别为0.9997、0.9993、0.9998、0.9994。4组分平均回收率分别为99.2%、101.2%、98.8%、99.2%,相对标准偏差(RSD)分别为0.60%、1.02%、0.62%、0.57%(n=3)。该方法准确、简便,适合上述4种有效成分的同时测定。     

苦参配方颗粒的高效液相色谱指纹图谱研究及定量分析

研究了苦参配方颗粒的指纹图谱和含量测定。采用高效液相色谱法,在C18柱上以乙腈-磷酸氢二钠水溶液(20 mmol/L,磷酸调pH 7.1)进行梯度洗脱,柱温35℃,检测波长220 nm,用指标成分氧化苦参碱、氧化槐果碱和苦参碱进行了定位,并在同一色谱条件下同时测定了它们的含量。确定了15个共有峰,其中7、8和11号峰分别为氧化苦参碱、氧化槐果碱和苦参碱。10批样品平均相似度为0.99以上,三个成分的含量分别为:氧化苦参碱50.0~79.8 mg/g;氧化槐果碱13.5~18.1 mg/g;苦参碱16.5~30.1 mg/g。结果表明:指纹图谱与指标成分含量测定相结合,可提高苦参配方颗粒的内在质量控制水平。     

高效液相色谱法测定贯叶连翘中的4种成分

本文利用高效液相色谱法同时测定中药贯叶连翘中绿原酸、芦丁、金丝桃苷和槲皮素四种成分的含量。采用Tiahhe Kromasil C18 100 A(5μm,250mm×4.6 mm)反相色谱柱;流动相为V(乙腈)∶V(水)=20∶80(含0.02%三氟乙酸);紫外检测波长270nm;流速1.0 ml/min;柱温40℃。绿原酸、芦丁、金丝桃苷和槲皮素线性范围分别为3.4~34μg.mL-1(r=0.9993),1.8~18μg.mL-1(r=0.9998),2.3~23μg.mL-1(r=0.9999),3.5~35μg.mL-1(r=0.9991),平均回收率(n=5)分别为98.4%(RSD=1.48%),101.8%(RSD=0.74%),103.7%(RSD=0.77%),103.5%(RSD=1.28%)。方法线性范围宽、相对标准偏差低、精密度高、重现性好,应用于贯叶连翘及制剂样品的测定,结果令人满意。     

多波长自动融合指纹图谱策略及其在蜂胶质量评价中的应用

提出了一种简化数据处理过程的多波长自动融合指纹图谱策略,并应用于蜂胶乙醇提取物的质量评价。运用超高效液相色谱（UPLC）技术对5个厂家的15批蜂胶乙醇提取物进行220、245、270、320 nm的多波长检测。样品采用Agilent Poroshell 120 EC-C18(3 mm×100 mm,2.7μm)色谱柱进行分离;以甲醇-0.2%磷酸水溶液为流动相进行梯度洗脱。利用“中药色谱指纹图谱相似度评价系统”进行全峰匹配,实现了每个样品多个波长下各色谱峰数据的自动融合。以270 nm单波长为对照,比较其与多波长融合在共有色谱峰、相似度评价、聚类分析、主成分分析方面的差异。蜂胶多波长融合指纹图谱包含33个特征峰,其中14个特征峰可定性,分别为咖啡酸、ρ-香豆酸、阿魏酸、异阿魏酸、3,4-二甲氧基肉桂酸、肉桂酸、槲皮素、山奈素、芹菜素、异鼠李素、乔松素、白杨素、高良姜素、咖啡酸苯乙酯。各批次特征峰保留时间的相对标准偏差（RSD）均小于1.00%,峰面积RSD为14.39%～112.02%,平均值为37.94%。15批蜂胶融合指纹图谱的相似度为0.902～0.994,主成分分析、聚类分析均...     

液相色谱特征图谱用于草乌成分定量

测定不同产地草乌的液相色谱指纹图谱,构建草乌的特征图谱,对不同草乌样品进行相似性对比分析,考察不同产地草乌的生物碱总量含量差异.采用色谱柱为WelchromC18柱(250 mm×4.6 mm,5μL),流动相为甲醇–0.1％三乙胺(体积比为75:25),流量为1 mL/min,检测波长为235 nm,柱温为30℃,进样体积为20μL.对10个批次样品进行相似度分析和含量测定,确定草乌的特征图谱共有模式,标定10个特征峰,指认了新乌头碱、乌头碱、次乌头碱的特征峰.10批不同产地草乌的相似度均大于0.90,相似度较好.产地1的草乌总生物碱含量为3.4046 mg/g,在10个产地中含量最高.其它产地草乌总生物碱含量相近.     

鱼腥草中黄酮类成分的高效液相色谱指纹图谱分析

采用均匀实验设计和信息理论评价方法,建立了鱼腥草中黄酮类成分的高效液相色谱(HPLC)指纹图谱的分析方法。采用建立的方法和本研究室提出的指纹图谱评价软件,对同样种植条件下10个批次的鱼腥草指纹图谱进行了相似性评价,相似度均大于0.90;同时测定了芦丁、槲皮甙和槲皮素3个成分在10批鱼腥草药材中的含量分别为0.25%～0.34%、0.27%～0.37%、0.012%～0.016%。另外对不同采收季节和不同部位的鱼腥草药材中的黄酮类成分进行了指纹图谱的测定、主成分分析以及成分含量测定,结果表明,不同季节、不同部位的鱼腥草中黄酮类化合物的指纹图谱及成分含量存在较大的差异,且药用部位的差异大于采收季节的差异。该方法为规范鱼腥草中黄酮类成分在制药和用药的实际应用提供了一些可靠的基础信息。     

葛根芩连配方颗粒标志性成分含量分析及指纹图谱研究

采用反相高效液相色谱法-二极管阵列检测器,以甲醇-水(内含1%三乙胺、1%乙酸,用磷酸调pH至3)为流动相,对中药复方制剂葛根芩连配方颗粒中3种主要标志性成分的含量同时分析测定,并采用相同的流动相对其指纹图谱进行研究。实验结果显示,3种主要标志性成分葛根素、黄芩苷和小檗碱在含量分析测定条件下,各组分分离良好,相关系数均为0.9999,线性范围分别为0.042~1.05、0.13~3.25和0.060~1.50μg,加样回收率在95%~106%之间;在指纹图谱研究中,以黄芩苷为参照物峰,标定了32个共有峰,分析的11批葛根芩连配方颗粒与共有模式之间具有良好的相似性,相似度均在0.9以上。建立的含量测定及指纹图谱分析方法灵敏度高、专属性强,可用于葛根芩连配方颗粒的质量控制。     

邓老凉茶颗粒的超高效液相色谱质谱联用指纹图谱研究

建立了适用于邓老凉茶颗粒质量控制的超高效液相色谱质谱联用指纹图谱分析方法。样品采用甲醇索氏萃取60 min,萃取液采用超高效液相色谱质谱法进行指纹图谱分析。色谱柱采用Waters ACQUITY HSST3 C18(150 mm×3.0 mm,1.8μm),以0.5%甲酸-乙腈为流动相进行梯度洗脱,流速为0.8 mL/min,柱温35℃。质谱采用负离子ESI模式,选择基峰离子流质量色谱图进行指纹图谱研究。32个共有峰在15 min内得到良好分离,其中15个共有峰通过对照品进行了确证。通过《中药色谱指纹图谱相似度评价系统2004A版》对邓老凉茶颗粒样品进行相似度分析,15个批次样品的相似度均达到0.960以上,表明邓老凉茶颗粒的产品质量稳定性很好。以32个共有峰的相对峰面积进行主成分分析,邓老凉茶颗粒样品之间的细微质量差异得到明显区分。该方法快速、高效、可靠,可有效地用于邓老凉茶颗粒的质量控制。     

基于牛舌草指纹图谱的多指标成分相对定量与鉴别方法

色谱指纹图谱法在中草药产地鉴别或中成药鉴别中发挥着重要作用,然而色谱峰强度和位置易受目标物提取和分离条件的影响,发展更加准确的指纹图谱具有重要意义。该文以色谱峰中某一个常见组分（芦丁）作为内标,分析其他组分的相对含量,以相对含量作为指纹图谱信息,结合化学模式识别可以精确给出产地的相似度。以牛舌草的液相色谱指纹图谱指纹峰为例,以其中芦丁的组分峰作为基准峰,其他指纹峰以芦丁为参照,计算每个指纹峰以芦丁计的含量,建立了牛舌草的指纹图谱。将获得的相对含量指纹图谱采用系统聚类分析和主成分分析进行化学模式识别研究,实现了不同产地牛舌草的区分。该方法建立了牛舌草多指标成分的相对定量与鉴别方法,既节省资源,又具有可操作性,对于其他中药或中成药的质量控制具有一定的借鉴意义。     

A novel method for quality consistency evaluation of Glycyrrhiza formula granules based on a spectrum-effect study

Quality consistency of Glycyrrhiza formula granules is essential for guaranteeing clinical efficacy. However, a suitable method to accurately and conveniently evaluate the consistency of the clinical efficacy of Glycyrrhiza formula granules is currently not available. This study established a method for the simultaneous determination of 12 active components in Glycyrrhiza formula granules using ultra-high-performance liquid chromatography coupled with quadrupole-time-of-flight tandem mass spectrometry. The rate of inhibition of cyclooxygenase-2 by different batches of Glycyrrhiza formula granules was determined. Near-infrared spectra were collected for different batches of Glycyrrhiza formula granules to detect their biological activity in the inhibition of cyclooxygenase-2. The quality consistency of the 11 batches of Glycyrrhiza formula granules was evaluated using principal component and correlation analyses. The results showed significant differences in the formula granules of Glycyrrhiza uralensis produced by the different manufacturers. Some differences were also observed among batches of formula granules produced by the same manufacturer. Correlation analysis of the chemical components and cyclooxygenase-2 activity showed that glycyrrhizic acid, liquiritin, and isoliquiritin were the main active components of Glycyrrhiza. Correlation analysis of the near-infrared spectra and cyclooxygenase-2 inhibition activity showed a high correlation between the active components and three characteristic bands: 3383–3995, 4227–4651, and 5315–5878 cm⁻¹. In this study, the main active anti-inflammatory components of Glycyrrhiza granules were screened. Thus, the near-infrared spectrum and characteristic active band of multi-index active components can be used to quickly detect the quality consistency of Glycyrrhiza formula granules, thereby improving the ability to control the quality and consistency of these granules.     

一测多评法在舒肝益脾颗粒中的应用

建立了舒肝益脾颗粒一测多评(QAMS)的高效液相色谱(HPLC)测定方法,并验证该方法在质量控制中的适用性与准确性.该方法能较好地分离舒肝益脾颗粒中3种主要成分(五味子醇甲、五味子甲素、五味子乙素),并以五味子醇甲为内参物,建立五味子甲素、五味子乙素与其之间的相对校正因子(fs/k),用fs/k计算各代表性成分含量,实...     

纳米金增强低温等离子体离子化质谱快速检测苯胺

低温等离子体(Low-temperature plasma,LTP)作为敞开式离子源满足环境检测要求的样品原位、快速检测,然而水体的基体效应使得检测灵敏度不足。该文将金纳米颗粒溅射于针灸针表面后,结合低温等离子体离子源进行检测,实现了质谱信号的增强效应,可以快速灵敏检测水体中的苯胺。结果表明,相比于无纳米金修饰的针尖,苯胺检测信号强度增强了43倍,且具有较低的背景噪音。苯胺的质量浓度与质谱信号强度在1~50μg/L范围内呈线性关系,检出限(LOD)为0.64μg/L,每个样品检测时间约为1 min。该方法简单易操作,结合便携式质谱有望用于环境水体及突发性水源污染事件中苯胺的检测。     

丹荷颗粒治疗高脂血症质量标志物发现研究

为寻找丹荷颗粒治疗高脂血症的质量标志物,该研究基于丹荷颗粒体内成分分析结果,采用Cyto-scape软件构建高脂血症-共有靶点-丹荷颗粒体内成分作用网络,利用DAVID及String数据库分别对共有靶点进行生物过程、通路富集及网络拓扑分析,明确丹荷颗粒降脂作用关键靶点及成分,再建立油酸诱导的HepG2细胞脂质堆积模型验...     

Qualitative and quantitative analyses of aloe-emodin,rhein, and emodin in qi yin granules by high-performance thin-layer chromatography

The aim of this study was to perform qualitative and quantitative analyses of aloe-emodin, rhein, and emodin in three prepared samples of compound qi yin granules by high-performance thin-layer chromatography (HPTLC) and to establish an analytical method. TLC was used to qualitatively analyze the three major components of the compound: aloe-emodin, rhein, and emodin. HPTLC was performed to determine the contents of the three components. HPTLC analysis showed that using Anhui Liangchen high-efficiency silica gel G plate was the optimal stationary phase and the upper layer solution of a petroleum ether–ethyl acetate–formic acid (15.5:5:1, V/V) mixed solution was the optimal developing agent. The composition of the samples for testing was basically the same, but the content was different. In summary, this study used HPTLC to qualitatively and quantitatively analyze aloe-emodin, rhein, and emodin in compound qi yin granules. It can lay the foundation for improving the quality control and standards of compound qi yin granules.

     

Film-forming synthetic polyelectrolytes for phosphogypsum modification

Methods for deposition of film-forming water-insoluble polycomplexes onto the surface of granulated phosphogypsum were developed. The effect of the resulting films on the physicochemical and performance characteristics of the phosphogypsum granules containing crystalline solvates of calcium sulfate was examined, as well as on leaching from the granules of various admixed components.     

养血清脑颗粒的高效液相色谱指纹图谱研究

采用变换波长检测法建立了养血清脑颗粒HPLC指纹图谱,确定了35个共有色谱峰在药材中的归属,并用液相色谱-质谱联用(LC-MS/MS)法鉴定出部分化学成分,同时对制剂中的4种指标性成分进行了定量检测.结果表明,制剂与药材具有良好的色谱峰相关性,4种指标性成分在各自的浓度范围内线性关系良好(r＝0.9997～0.9999...     

Modification of phosphogypsum granules by humic acids

Methods for introducing humic acid into granular multicomponent phosphogypsum-based ameliorants are elaborated. The influence of modifying additives of humic acids on the physicochemical and performance characteristics of phosphogypsum granules containing crystalline solvates of calcium sulfate, and on the process of leaching different extrinsic components from the granules, were studied.     

An integrated approach of high-performance liquid chromatography–mass spectrometry-based chemical profiling,network pharmacology,and molecular docking to reveal the potential mechanisms of Qishen Gubiao granules for treating coronavirus disease 2019

Qishen Gubiao granules, a traditional Chinese medicine preparation composed of nine herbs, have been widely used to prevent and treat coronavirus disease 2019 with good clinical efficacy. In the present study, an integrated strategy based on chemical profiling followed by network pharmacology and molecular docking was employed, to explore the active components and potential molecular mechanisms of Qishen Gubiao granules in the therapy of coronavirus disease 2019. Using the ultra-high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry technique, a total of 186 ingredients corresponding to eight structure types in Qishen Gubiao preparation were identified or structurally annotated with the elucidation of the fragmentation pathways in the typical compounds. The network pharmacology analysis screened 28 key compounds including quercetin, apigenin, scutellarein, luteolin and naringenin acting on 31 key targets, which possibly modulated signal pathways associated with immune and inflammatory responses in the treatment of coronavirus disease 2019. The molecular docking results observed that the top 5 core compounds had a high affinity for angiotensin-converting enzyme 2 and 3-chymotrypsin-like protease. This study proposed a reliable and feasible approach for elucidating the multi-components, multi-targets, and multi-pathways intervention mechanism of Qishen Gubiao granules against coronavirus disease 2019, providing a scientific basis for its further quality evaluation and clinical application.     

Influence of specific gravity and food on movement of granules in the gastrointestinal tract of rats

The suitability of rats as an animal model for estimating the bioavailability of controlled-release granules in humans was investigated. Non-disintegrating granules (diameter of 0.8 mm; specific gravity of 0.9-1.85) were used as a model preparation. Twenty granules were administered to fed rats, fasted rats and rats given soft food, and the number of granules remaining in the gastrointestinal tract was counted at suitable intervals. Granules with a specific gravity of 1.25 administered to fasted rats were rapidly emptied from the stomach with a 50% gastric emptying time of 1 h as compared with granules with a specific gravity of less than 1.0 or with a high specific gravity such as 1.85. The presence of food in the stomach reduced the emptying rate of granules. The mean transit time of granules through the small intestinal tract was not influenced by the specific gravity or the presence of food. The mean transit time was about 3 h. It was found that the transit profile of granules through the gastrointestinal tract in rats was similar to that of granules in humans. Accordingly, it is possible to use rats at the preformulation stage for estimating the bioavailability of controlled-release granules in humans.