反相高效液相色谱法检测脂必妥片中洛伐他汀的含量

对脂必妥片样品进行预处理,得到的混合物用薄层色谱、反相高效液相色谱法进行定性、定量分析,建立检测其含量的方法。当色谱条件为色谱柱:Kromasil(C18250 mm×4.6 mm,5μm);流动相体积比:乙腈∶水为85∶15,;流速:1.0 ml.min-1;检测波长:420 nm;柱温:30℃;测定结果表明被测峰和其它峰可完全分离,在每毫升10.21~200.03μg内具有良好的线性关系,r=0.9997,测得其中洛伐他汀含量为0.25%,回收率:97.73%,RSD:0.56%。这种方法准确、可靠,可用于含洛伐他汀药品的质量控制。     

瑶药冷骨风质量控制方法研究

瑶药冷骨风来源于睡莲科植物萍蓬草(Nuphar pumilum)的干燥根茎,为瑶族人习用药材,具有止咳补虚、除蒸止汗、祛瘀调经、止血的作用,目前历版《中国药典》和地方标准并未有收载其质量控制方法。该研究收集了10批冷骨风药材,采用生药鉴别方法对冷骨风药材性状进行显微鉴别,用TLC(薄层色谱)法对药材进行定性鉴别,用高效液相色谱法对没食子酸含量进行测定。结果表明:(1)色谱柱为Welch Ultimate XB-C_(18)柱(4.6 mm×250 mm,5μm),流动相为甲醇-0.05%磷酸溶液(5∶95),流速为1.0 mL·min~(-1),检测波长为272 nm,柱温为室温。(2)建立了冷骨风药材性状、显微、TLC鉴别方法。(3)含量测定中没食子酸在0.072 1~0.360 5μg范围时,进样量与峰面积呈良好的线性关系,平均回收率为103.66%,RSD为2.03%(n=6)。(4)10批样品没食子酸含量为0.82%~1.23%,平均含量为0.94%。因此,建立的瑶药冷骨风质量控制方法具有较强的科学性,可用于冷骨风药材的质量控制。     

西藏产两种岩白菜中岩白菜素的HPLC测定

建立测定了岩白菜中岩白菜素含量的方法.色谱柱:WatersC18柱 5μm×3.9mm×150mm ,流动相:甲醇∶水∶磷酸=20∶80∶0.1,流速为1.0mL/min,检测波长275nm,AUFS0.01,柱温为室温.结果表明,岩白菜素在0.16～0.08μg有良好线性关系,r=0.9992,平均回收率为98.14%,RSD为1.12%.本方法是测定岩白菜中岩白菜素含量的快速、简便、准确可靠的定量方法.     

反相高效液相色谱法测定不同品种花椒中芦丁和槲皮素的含量

目的:建立RP-HPLC测定花椒中芦丁与槲皮素含量的方法,并对不同种花椒的中芦丁与槲皮素含量进行测定与比较。方法:Zorbax Eclipse C18色谱柱(150 mm×4.6 mm,5μm),流动相∶甲醇-0.4%磷酸(50∶50);流速1 mL/min;检测波长:360 nm;柱温25℃。结果:芦丁在0.25~5.0μg,r=0.999 9峰面积与质量浓度呈良好的线性关系;平均回收率为99.1%,RSD为4.3%(n=3)。槲皮素在0.25~0.5μg,r=0.999 9峰面积与质量浓度呈良好的线性关系;平均回收率为111.2%,RSD为5.1%(n=3)。结论:该方法可用于花椒中芦丁和槲皮素的测定。测定结果表明,韩城红花椒中芦丁含量最高,茂汉红花椒次之,四川青花椒较少,云南青花椒最低。槲皮素在韩城红花椒中含量较高,在其他三种花椒中差别不大。     

和中消滞合剂中总槲皮素的定性定量研究

目的建立和中消滞合剂中总槲皮素的定性定量方法。方法采用薄层色谱法定性,高效液相色谱法(HPLC)定量。色谱柱为Inertsil ODS-XP柱(4.6 mm×150 mm,5μm),流动相为甲醇-0.4%磷酸溶液(36∶64),检测波长360 nm,流速为1 ml·min~(-1),柱温为30℃。结果薄层色谱斑点清晰;HPLC的槲皮素进样浓度在0.039～0.413μg·ml~(-1)范围内,与峰面积值呈良好的线性关系,回归方程Y=46589X-4756(r=0.9999);平均加样回收率为98.10%,RSD=0.96%(n=6)。结论建立和中消滞合剂中总槲皮素的定性定量测定方法可行,可用于该制剂的质量控制。     

痹康颗粒的质量标准研究

目的:建立痹康颗粒的质量标准.方法:采用薄层色谱法对痹康颗粒中当归、丁香进行定性研究,并采用高效液相色谱法对方中补骨脂素、异补骨脂素进行含量测定研究.色谱柱:Agilent XDB-C18柱(4.6mm 150mm,5μm);流动相:甲醇-水(45:55);检测波长:246nm;流速:1.0ml/分钟;柱温:25℃.结果:薄层色谱斑点清晰,阴性无干扰;补骨脂素在浓度范围8.64～43.20mg/ml内呈良好的线性关系,r=0.9998,平均加样回收率为97.33%,RSD=1.08%(n=6);异补骨脂素在浓度范围8.92～44.60mg/ml内呈良好的线性关系,r=0.9997,平均加样回收率为98.38%,RSD=0.92%(n=6).结论:该方法简便、准确、可靠,可以作为痹康颗粒的质量控制方法.     

拔毒消炎软膏质量控制研究

目的研究拔毒消炎软膏的质量控制方法。方法用薄层色谱法(HPLC)对制剂中大黄、黄柏进行定性鉴别,高效液相色谱法测定大黄酚的含量。结果定性鉴别薄层色谱斑点特征明显;高效液相色谱法测定含量,大黄酚在0.061~0.304μg/ml范围内呈良好的线性关系(r=0.9954),平均加样回收率为98.68%,RSD=1.39%。结论采用薄层色谱法定性、高效液相色谱法定量,简便准确、重现性良好,可有效控制该制剂质量。     

HPLC法测定宁夏枸杞中法荜枝苷的含量

本文采用高效液相色谱法,建立宁夏枸杞中法荜枝苷的含量测定方法。色谱条件:Diamonsil C8柱(150mm×4.6 mm,5μm);流动相为A:乙腈-水-醋酸(5∶94.5∶0.5),B:乙腈-水-醋酸(72∶27.5∶0.5),梯度洗脱。流速:1 mL/min;柱温:30℃;检测波长:346 nm。结果表明,在0.1～10μg/mL范围内线性关系良好,相关系数r=0.9998(n=8)。法荜枝苷的平均回收率为99.1%,RSD为1.55%。该方法准确可靠,可用于测定宁夏枸杞中法荜枝苷的含量,为宁夏枸杞开发利用提供理论依据。     

RP-HPLC法测定芦笋中黄酮类化合物芦丁的含量

以芦丁标准品为对照,利用反相高效液相色谱法对芦笋中黄酮类化合物芦丁的含量进行定量测定。采用Agilent Eclipse XDB-C18色谱柱,柱温25℃,流动相由甲醇-水-磷酸(55∶44.5∶0.5)组成,流速为0.7 mL/min,检测波长390 nm。结果表明黄酮类化合物中各组分基线分离良好;进样量在0.07~0.7μg/20μL范围内,峰面积A与进样浓度C呈良好的线性关系,回归方程为A=1 5176C-10.388,相关系数R2=0.999 4;加样回收率为101.051%,RSD=3.306%;以保留时间和峰面积作精密度试验,RSD分别为0.199%和1.24%。该方法样品处理简单,准确度高,精密度好,适合于芦笋中芦丁含量的测定。     

陕西柑橘主产区13种推广品种维生素C含量分析

为了测定陕西柑橘主产地区13种推广种植的柑橘品种中维生素C含量,为陕西柑橘的生产、加工、育种研究提供实验数据,采用高效液相色谱法对13个柑橘品种的维生素C含量进行检测。检测条件为:色谱柱Diamonsil(钻石)C18柱(4.6mm×150mm,5μm);检测波长为245nm;流动相为甲醇∶0.1%磷酸=1∶99(V/V),等梯度洗脱;流速0.8mL·min-1;柱温:25℃,进样量10μL。实验结果表明,汉中13个主要推广种植的柑橘品(系)中,维生素C含量在234.07~392.92mg·kg-1之间,各品种之间维生素C的含量各不相同,差异显著。本研究的结果表明,汉中柑橘中维生素C含量较高,品质较好。     

The biotransformation of simple phenolic compounds by Brettanomyces anomalus

Abstract Brettanomyces anomalus is shown here to metabolise p -coumaric, caffeic and ferulic acid to 4-vinyl and 4-ethyl derivatives. We also demonstrate the transformation of vanillin to both vanillyl alcohol and vanillic acid by this yeast. The results presented here show the production of these compounds during the fermentation of this organism and also the effects of these and other simple phenolic compounds on the growth of the organism. The products were analysed and their identities were determined by TLC, HPLC and by mass spectrometry.     

薄层色谱和高效液相色谱联用测定暗纹东方鲀肌肉中肌肽和谷胱甘肽的含量

通过薄层色谱(TLC)与高效液相色谱(HPLC)联用技术鉴定了暗纹东方鲀(Takifugu obscurus)肌肉中存在肌肽和谷胱甘肽,同时利用高效液相色谱法测定了肌肽和谷胱甘肽(GSH)的含量。薄层层析采用的展开剂为正丁醇:乙酸:水(4∶2∶1),层析板为硅胶板。高效液相色谱利用Kromasil C18反相柱分析,流动相为10%的纯乙腈和90%含有0.05%三氟乙酸的超纯水。结果表明:通过薄层色谱和高效液相色谱鉴定了暗纹东方鲀肌肉中肌肽和谷胱甘肽,其中暗纹东方鲀肌肉中肌肽含量约213μg/g(鲜重),还原性谷胱甘肽含量约211μg/g(鲜重)。本法样品无需衍生,操作简便,适合于暗纹东方鲀肌肉中肌肽和谷胱甘肽的测定。本文为生物体内肌肽和谷胱甘肽的研究提供借鉴意义。     

微生物转化方法生产香草酸与香草醛的初步研究

从实验室保藏的菌种中筛选到一株黑曲霉（Aspergillus niger）SW-33,能够将1g/L的阿魏酸底物转化为0.23g/L的香草酸,相应的摩尔转化率为29.35％;流加四次底物阿魏酸后,产物浓度达到1.11g/L,相应的摩尔转化率为44.9％。为了提高产物浓度,对培养基和发酵条件进行优化,使得该菌株能够将1g/l的阿魏酸底物转化为0.46g/L的香草酸,相应的摩尔转化率为57.81％。提取得到的香草酸,经HPLC测定,纯度为85.9％;提取收率为75.2％。用含香草酸的转化液,或者用提取的结晶香草酸,加入朱红密孔菌（Prcnporus cinnabarnus）SW-0203发酵培养液,可得到转化产物香草醛。     

小儿感冒茶的薄层鉴别和定量测定研究

目的为制定小儿感冒茶(山银花、板蓝根、重楼)的质量控制方法。方法用TCL鉴别山银花、板蓝根、重楼。用高效液相色谱法测定小儿感冒茶中绿原酸的含量。结果通过方法学考察,绿原酸检测浓度在0.244~1.952μg范围内与峰面积积分值呈良好的线性关系,加样回收率为99.22%,RSD%=0.92(n=2)。结论实验应用方法简便准确、重现性好、精密度高。所建质量标准可用于小儿感冒茶的质量控制。     

Candida galli Strain PGO6: A Novel Isolated Yeast Strain Capable of Transformation of Isoeugenol into Vanillin and Vanillic Acid

Candida galli strain PGO6 isolated from oil-contaminated water is the first isolated yeast strain which is capable to form vanillin and vanillic acid during isoeugenol biotransformation. The products were confirmed by thin-layer chromatography (TLC), changes in the UV absorption pattern and high-performance liquid chromatography (HPLC). The phenotypic and physiochemical characteristics as well as molecular phylogenetic analysis based on amplification the ITS1-5.8S-ITS2 rDNA regions indicated the isolated strain PGO6 was identified as C. galli (GenBank accession number HM641231). Resting cells of C. galli PGO6 from the late-exponential of growth phase were used as biocatalysts for the biotransformation of isoeugenol. The optimal molar conversion of vanillin (48%) and vanillic acid (19%) was obtained after a 30 h incubation using 0.1% (v/v) of isoeugenol and 6 mg of dry weight of cells per ml without further optimization. Under these conditions, the total amount of vanillin and vanillic acid was 583 mg l(-1). Further biotransformation was carried out using 0.5% (v/v) of isoeugenol under the resting cells conditions, yielding a vanillin concentration of 1.12 g l(-1) (molar yield 25.7%) after 60 h incubation. This study brings the first evidence for biotransformation of isoeugenol to vanillin and vanillic acid by a yeast strain.     

Pseudomonas resinovorans SPR1, a newly isolated strain with potential of transforming eugenol to vanillin and vanillic acid

In this study a novel strain was isolated with the capability to grow on eugenol as a source of carbon and energy. This strain was identified as Pseudomonas resinovorans (GenBank accession no. HQ198585) based on phenotypic characterization and phylogenetic analysis of 16S rDNA gene. The intermediates coniferyl alcohol, coniferyl aldehyde, ferulic acid, vanillin and vanillic acid were detected in the culture supernatant during eugenol biotransformation with this strain. The products were confirmed by thin layer chromatography (TLC), high performance liquid chromatography (HPLC) and spectral data achieved from UV-vis, FTIR and mass spectroscopy. Using eugenol as substrate and resting cells of P. resinovorans SPR1, which were harvested at the end of the exponential growth phase, without further optimization 0.24 g/L vanillin (molar yield of 10%) and 1.1g/L vanillic acid (molar yield of 44%) were produced after 30 h and 60 h biotransformation, respectively. The current work gives the first evidence for the eugenol biotransformation by P. resinovorans.     

酚酸类物质对三七幼苗的化感影响

该文研究了不同浓度的阿魏酸、对香豆酸、丁香酸、对羟基苯甲酸、香草酸5种酚酸类物质对三七幼苗生长和生理的影响。结果表明:处理后,三七幼苗的苗高、根长、可溶性蛋白质含量、根系活力、CAT以及POD活性均有所降低。其中,阿魏酸各处理组幼苗的苗高及POD活性均显著降低,50、100 mg·L~(-1)的对香豆酸以及100 mg·L~(-1)的香草酸处理组幼苗苗高也分别比对照显著降低16.19%、16.67%和29.29%;对香豆酸、丁香酸以及对羟基苯甲酸各处理组幼苗根长均显著低于对照;香草酸处理组幼苗的根系活力也显著低于对照,且幼苗的CAT活性在10、50、100 mg·L~(-1)丁香酸、对羟基苯甲酸以及香草酸处理下也达到了显著降低水平。此外,1 mg·L~(-1)阿魏酸以及100 mg·L~(-1)香草酸处理组幼苗的叶绿素含量也均显著降低;中高浓度的阿魏酸、对香豆酸、丁香酸、对羟基苯甲酸增加了三七幼苗的MDA含量,而香草酸在0.1、1、10、100 mg·L~(-1)浓度下显著降低幼苗的MDA含量;丁香酸、香草酸、对羟基苯甲酸以及中高浓度的对香豆酸增加了三七幼苗的SOD活性,且香草酸各处理组均达到了显著性水平。综上结果表明,5种酚酸类物质对三七幼苗均具有一定的化感抑制作用,但各酚酸物质的作用方式及强度并不完全一致,阿魏酸的化感影响较大,这为进一步研究三七的化感自毒作用提供了一定的理论参考。     

HPLC示差折光法测定藻油中DHA的含量

首次采用HPLC示差折光法测定藻油中DHA的含量。色谱柱为Eclipse XDB-C18(Analytical 4.6×250mm,5μm),流动相为乙腈∶四氢呋喃∶水(含0.4%HAC)=77∶3∶20,柱温为30℃,流速为1.0 mL/min。该条件下DHA在0.259～6.225 mg/mL内呈良好的线性关系,相关系数R2=0.9995,平均回收率为101.15%,RSD为1.98%(n=6)。该方法可靠、简便、重现性好,可作为藻油中DHA的定量方法。     

High-performance liquid chromatography separation of phospholipid classes and arachidonic acid on cyanopropyl columns

An HPLC method for the separation and analysis of arachidonic acid and eight phospholipid classes is described: phosphatidylglycerol, phosphatidylinositol, cardiolipin, phosphatidylserine, phosphatidylethanolamine, phosphatidylcholine, sphingomyelin, and 2-lysophosphatidylcholine. The separation is carried out at 60 degrees C on 2 cyanopropyl columns using a gradient of acetonitrile and 5 mM sodium acetate (pH 5.0). Cyanopropyl columns require a lower proportion of water in the mobile phase to elute the more polar phospholipids than other types of columns and are thus less prone to equilibration problems. The method is highly reproducible (average coefficient of variation for each retention time less than or equal to 3.5%) and permits analysis of peaks by phosphorus content. Data obtained by analyzing lipid extracts from rat alveolar macrophages prelabeled with [G-3H]-arachidonic acid were analyzed by this HPLC method and compared to standard analysis by TLC. There was a significant correlation between the radioactivity profiles obtained with the two chromatographic methods (HPLC versus TLC) by linear regression analysis [HPLC = 0.83 (TLC) + 3.58, n = 25, r = 0.95, P less than 0.001].     

银耳多糖单糖组成分析的三种色谱方法比较

为选择一种准确快捷的方法测定银耳多糖的单糖组成,对薄层色谱法(TLC)、气相色谱法(GC)、高效液相色谱法(HPLC)三种色谱方法进行比较。结果表明,前两种方法的测定结果均不理想,而HPLC法,操作简便,灵敏度高,分离效果好,信息完整。测定结果为由葡萄糖、甘露糖、葡萄糖醛酸、木糖、岩藻糖组成,其摩尔比为0.24∶1.00∶0.06∶0.29∶0.25。HPLC法对酸性杂多糖组成糖分析是一种比较理想的选择。