高效液相色谱法快速测定银杏叶提取物中的萜类内酯

 394-397 -------------------------------------------------------------------------------- 建立了液-液萃取后高效液相色谱法（HPLC）测定银杏叶提取物（EGb）中萜类内酯含量的快速方法。EGb样品溶于体积分数为30%的乙醇溶液后用乙醚萃取,有机相浓缩后的残留物以HPLC分析,组分的分离采用C18柱,以甲醇-水-磷酸(体积比为25∶75∶0.1)为流动相,示差检测器检测。结果表明,样品净化程序较已报道的方法更简便,选择性强、快速（少于20 min）。该方法回收率大于99.0%、相对标准偏差小于2.0%、重现性好,可有效地用于银杏叶提取物的产品质量评价。     

用高效液相色谱法分析银杏黄酮时几个问题的探讨

研究了用高铲液相色谱法分析银杏叶的中黄酮含量时几个主要环节的操作条件,包括水解液组成,水解温度和时间,论证了在３７０ｎｍ波长下检测时,可用槲皮素下标准物质方便地求出桷皮素,山萘酚和异鼠纱３种黄酮的含量。水解液是５．５％ＨＣｌ甲醇庆８５￣９０℃回流１．３ｈ。采用Ｂｉｏ－ＳｉｌＯＤＳ５μｍ柱,１５０×４．０ｍｍＩ．Ｄ。,甲醇／０．４％磷酸水溶液（５７：４２）流动相,ＵＶ－３７０ｎｍ检测。上率和分析精度     

高效液相色谱法测定银杏叶提取物中槲皮素的含量

An HPLC method has been developed for the determination of quercetin,one of flavones,in extract ofGinkgo b1loba L,leaves.Quercetin was separated completely on a Zorbax-ODS column, 250mm× 4. 6mm i.d.,using a mixture of methanol, water and phosphoric acid(55:44. 6:0.4)as mobile phase; with UV detec-tion at 254nm. The results have shown that the recoveries were between 93.3～103.3%andCVwas l.4l%。     

Determination of the Flavonoids from Ginkgo Biloba Extract by High Performance Liquid Chromatography

Today Ginkgo biloba extract (GBE) is one of the most widely used food supplements and herbal medicines. The amounts of flavone glycosides, one of the key active components in GBE, vary according to the source of the ginkgo leaves and the extraction and enrichment procedures used to prepare the extract. A typical GBE contains from 22% to 27% of flavone glycosides. Ginkgo flavone glycosides are a group of small complex molecules that can be hydrolyzed to give kaempferol, quercetin and isor…     

反相银化高效液相色谱法测定银杏叶中银杏酚酸(英文)

 建立了反相银化高效液相色谱测定银杏叶中银杏酚酸含量的分析方法。在样品的浸提液中加入少量酸性盐溶液和吸附剂后 ,用一步反萃取法净化样品 ,有机相浓缩后供HPLC分析。流动相 :V(甲醇 )∶V(体积分数为 5 %的乙酸水溶液 ) =90∶10 ,其中银离子浓度 0 0 3mol·L-1,紫外检测波长 310nm。结果表明 4种银杏酚酸之间达到基线分离 ,该方法平均回收率为97 3% ,相对标准偏差 1 6 % ,最低检测量 0 0 2 6 μg ,可有效地用于银杏叶及其提取物中银杏酚酸的定量分析。     

Assay of 44 compounds in the cortex and xylem from roots and branches of Ginkgo biloba L. by ultra high performance liquid chromatography coupled with tandem mass spectrometry and chemometric analysis

The leaves of Ginkgo biloba L. have received much attention, whereas there has been little systematic analysis of the cortex and xylem from roots and branches. A comprehensive evaluation of the 44 compounds in the cortex and xylem would thus be of value to fully understand the potential medicinal properties of roots and branches. An assay of amino acids, terpene lactones, flavones, and phenolic acids was accomplished using ultra high performance liquid chromatography with tandem mass spectrometry. All of the calibration curves showed good linear regression (R² > 0.9902) within the tested ranges. The intra‐ and interday precision was less than 4.9% and the accuracy was within ±6.8%. The amount of terpene lactones in the cortex was 1.75–2.07‐fold higher than that in the leaves. The amount of glutamine (360 μg/g) in the taproot xylem was 2.64‐fold higher than that in the leaves (136 μg/g). Principal component analysis decreased in the order leaves > taproot cortex > rootlet > laterals cortex > branch cortex > stem cortex > taproot xylem > branch xylem > laterals xylem > stem xylem. The taproot of G. biloba might provide a supplementary source of terpene lactones, especially ginkgolide A and C, and of glutamine.     

高效液相色谱-蒸发光散射检测法测定烟草中的水溶性糖

采用Waters高效糖分析柱,梯度洗脱分离,建立了高效液相色谱-蒸发光散射检测法（HPLC—ELSD）同时测定烟草中水溶性糖的新方法。乙腈-水为流动相,流速1．0mL／min,柱温30℃,蒸发光散射检测器漂移管温度80℃,氮气作载气,流速2．00L／min。水溶性糖的线性范围：鼠李糖、果糖、葡萄糖、蔗糖0．5—30μg,检出限低于12．5ng;木糖、阿拉伯糖、甘露糖、麦芽糖0．5—20μg,检出限低于25．0ng。8种水溶性糖的加标回收率范围为86．0％～102．4％;相对标准偏差（n=5）皆小于4．1％。     

Isolation and enrichment of Ginkgo biloba extract by a continuous chromatography system

In this study, an effective method was developed for the isolation and enrichment of Ginkgo biloba extract by continuous chromatography system. The adsorption and desorption ratio of flavonoids as main index, the best macroporous resin was screened out from six resins by static adsorption and desorption tests. At the same time the adsorption and desorption parameters were optimized by dynamic adsorption and desorption tests. Under optimal parameters, five operations consisting of loading, washing, desorbing, regenerating, and balancing were integrated across the continuous chromatography system for the purpose of refining 66 L of crude extract solution. The results were as follows, 198.22 g of Ginkgo biloba extracts was produced, which contained 65.83 g of flavonoids and 15.44 g of lactones. The content of flavonoids and lactones increased from 2.76 and 0.72% in the crude extract to 33.21 and 7.79%, with a recovery yield of 91.26 and 81.21%. Methodology validation showed that the proposed method had high stability and reproducibility. Compared with the traditional macroporous resin method, the proposed method had a short processing time and low solvent consumption. Our studies indicated that the newly developed method is an effective procedure for the isolation and enrichment of Ginkgo biloba extract.     

银杏叶提取物中黄酮类成分的高效液相色谱分析

Quantitative reversed-phase high performance liquid chromatographic method has been developed for theseparation and determination of the flavonoids found in the extracts of the leaves of ginkgo biloba L. (EGb).Procedure includes hydrolysis of the flavonoids and subsequent quantitative chromatographic assay of the ob-tained aglycones on a C_(18) column with methanol-0.4% orthophosphoric acid (55:45) as eluent. The detec-tion was effected at 360nm.     

高效液相色谱法测定茯苓皮的指纹图谱

本文用正交设计优化茯苓皮的超声提取条件,并有效提取了茯苓皮药材内的主要成分三萜类物质,同时利用高效液相色谱法(HPLC)建立了提取物的液相指纹图谱。实验考察了不同提取溶剂、提取条件对提取工艺的影响;确立了最佳色谱条件,得到了茯苓皮中24种总提取物的指纹图;同时对10种不同产地的茯苓皮药材进行分析,标定了17个共有峰。研究结果表明,HPLC指纹图谱方法重现性好,稳定可靠,可用于控制茯苓皮中三萜成分的质量。     

高效液相色谱仪蒸发光散射检测器校准用标准物质的选择

对高效液相色谱蒸发光散射检测器(ELSD)校准用标准样品蔗糖–甲醇溶液和对乙酰氨基酚–甲醇溶液进行了研究。实验表明,用蔗糖–甲醇溶液和对乙酰氨基酚–甲醇溶液校准具有ELSD的高效液相色谱仪,其保留时间、峰面积、最低检测浓度3个参数均符合检定校准用标准物质要求。但蔗糖–甲醇溶液色谱峰的对称性差且响应值明显低于对乙酰氨基酚–甲醇溶液,因此用后者作为ELSD检校用标准物质更适合。     

应用高效液相色谱-二极管阵列检测器-蒸发光散射检测器联用技术同时测定清开灵注射液中的五类有效成分

建立了复方清开灵注射液中5类主要有效成分的定量测定方法。应用高效液相色谱-二极管阵列检测器-蒸发光散射检测器联用技术(HPLC-DAD-ELSD),根据各类成分紫外吸收光谱的差异,分别在240,254,280和330 nm波长下检测栀子苷、核苷(包括尿苷和腺苷)、黄芩苷和有机酸(包括绿原酸和咖啡酸)等4类成分,同时使用ELSD测定胆酸、熊去氧胆酸和猪去氧胆酸等3种甾体化合物,从而实现了清开灵注射液中5类有效成分(共9个化合物)的同时分离和定量测定。用该法测定了3个不同厂家的19批清开灵注射液成品。该法快速、准确,操作相对简单,为中药复方复杂体系的多组分定量测定和质量控制提供了一种可靠、合理且简便、易行的方法模式。     

反相高效液相色谱法制备银杏叶中聚戊烯醇同系物单体

利用制备高效液相色谱法从银杏叶中分离制备了聚戊烯醇同系物单体。在HiQ sil C18柱上,以异丙醇-甲醇-正己烷-水(体积比为50∶25∶15∶4)为流动相,流速10 mL/min,采用等度洗脱方式,制备了8种化合物,经紫外光谱、红外光谱及质谱分析,确认它们分别为C70,C75,C80,C85,C90,C95,C100和C105聚戊烯醇,其中主要成分为C85及C90聚戊烯醇。高效液相色谱分析表明,制备的C75C105聚戊烯醇化合物的纯度均在96%(质量分数)以上。在该色谱条件下,各色谱峰达到了基线分离,     

全二维液相色谱串联质谱用于银杏叶提取物成分分析的研究

建立了全二维液相色谱串联质谱分离分析模式,将质脂体色谱柱和ODS反相色谱柱作为二维分析色谱柱,二者通过一个连有两个0.5 mL定量环的八通阀耦联。质脂体色谱柱上的馏分在反相色谱柱上分离后,直接进入紫外-检测器,然后经分流器分流后进入大气压电离质谱。将该体系用于银杏叶提取物的组成研究,共检测到至少41个组分,结合紫外-可见光谱和质谱信息,其中13个组分初步鉴定为银杏内酯B、银杏内酯C、白果内酯、槲皮素芸香糖苷、槲皮素、槲皮素-3-O-β-D-葡萄糖基(1-2)-α-L-鼠李糖苷、槲皮素-3-O-β-D-葡萄糖苷、异鼠李素、山柰酚-3-O-β-D-芸香糖基(1-2)-α-L-鼠李糖苷、异鼠李素-3-O-β-D-芸香糖苷、山柰酚-3-O-β-D-葡萄糖苷、山柰酚和山柰酚-3-O-β-D-芸香糖苷。     

高效液相色谱法测定银杏果中有机酸的含量

建立了反相高效液相色谱测定银杏果中有机酸含量的方法.方法采用ultimate-C18色谱柱,以pH=2.0的磷酸盐缓冲溶液为流动相,流速0.5 mL/min,检测波长210 nm,在22 min内实现了7种有机酸的基线分离.有机酸的检出限在0.001～0.067μg/mL之间.所建立的方法具有分析速度快、线性范围宽、灵...     

Isolation and purification of ginkgo flavonol glycosides from Ginkgo biloba leaves by high-speed counter-current chromatography

A high-speed counter-current chromatography method was developed for the separation and purification of bioactive flavonol glycosides from a crude ethanol extract of Ginkgo biloba leaves. The separation was performed with a two-phase solvent system composed of n-hexane-butanol-ethyl acetate-methanol-0.5% acetic acid (1:0.5:3.5:1:4, v/v) and three pure compounds were eluted in high purities in a one-step separation. Their purities were determined by HPLC and identified by MS,(1)H-NMR, and(13)C-NMR.     

反相高效液相色谱-二极管阵列检测同时测定去痛片中4组分的含量

建立了一种同时测定去痛片中 4组分的含量的反相高效液相色谱法。采用YWGC1 8柱 ,以甲醇 磷酸二氢钠 (35∶6 5 )为流动相 ,流速为 1.0mL min ,用二极管阵列检测器检测 ,检测波长为 2 14nm。该方法简便快捷 ,线性范围广 ,结果准确可靠 ,用于实际样品的测定 ,结果满意。     

高效液相色谱/蒸发光散射法测定多黏菌素类原料药中主成分含量

建立了高效液相色谱/蒸发光散射法测定多黏菌素B和多黏菌素E原料药中主成分含量的分析方法。采用Phenomenex Kinetex Biphenyl色谱柱(50 mm×4.6 mm i.d.,5μm)分离,甲醇和20 mmol/L乙酸铵水溶液(含0.6%甲酸)为流动相,梯度洗脱,流速为0.5 mL/min;蒸发光散射检测器参数为:漂移管温度55℃,气体压力20 psi,增益250。结果表明,多黏菌素B和多黏菌素E在10～200μg/mL质量浓度范围内线性良好,检出限分别为0.8μg/mL和1.2μg/mL,定量下限分别为2.6μg/mL和4.0μg/mL。批内回收率分别为100%～104%和101%～103%,批内相对标准偏差(RSD)分别为0.90%～2.4%和0.90%～2.6%,批间回收率分别为101%～103%和101%～102%,批间RSD分别为1.1%～1.9%和1.3%～1.7%。与微生物检定法相比,该方法简便,能够更准确地反映原料药中目标分析物含量,精密度更高,可用于多黏菌素B和多黏菌素E两种原料药的质量控制。     

高效液相色谱/蒸发光散射检测法同时测定饲料中12种甜味剂

建立了饲料中鼠李糖、木糖、果糖、葡萄糖、甜菊双糖苷、蔗糖、麦芽糖、乳糖、蔗果三糖、棉籽糖、蔗果四糖、水苏糖共12种甜味剂的高效液相色谱同时分离检测方法。采用XB-NH2柱分离,以乙腈-水为流动相梯度洗脱,蒸发光散射检测器进行测定。结果表明,12种甜味剂在0.05~5 g/L范围内均具有良好的线性关系,相关系数为0.996 3~1.000 0,检出限不大于0.04 g/L,方法的回收率为86.6%~112%,相对标准偏差(RSD)为0.5%~6.7%。该方法简单快速,定量准确可靠,适用于饲料中甜味剂的日常检测。     

高效液相色谱-蒸发光散射法测定牛黄中多种有效成分含量及其质量相关性研究

建立高效液相色谱-蒸发光散射法(HPLC-ELSD)同时快速测定牛黄中7种组分的含量的方法。色谱柱为UltimateAQ-C18柱,流动相为乙腈-0.2%甲酸水溶液,梯度洗脱,流速1mL/min;蒸发光散射检测器参数:漂移管温度100℃,载气(N2)流速1.9L/min。在选定色谱条件下,胆固醇、各种胆汁酸及其钠盐峰形良好且能达到很好地分离。各组分色谱峰峰面积的对数与浓度的对数呈良好线形关系(r0.9972);标准加入回收率为98.8%～112.7%;7种组分的最低检出限为0.001～0.007g/L。本方法可简便、快速地同时检测不同牛黄样品中7种组分的含量并可表征不同牛黄样品的质量,从而为该名贵药材的质量控制提供更全面的依据和参考。