Secondary metabolite credentials ofEvolvulus alsinoides by high performance thin layer chromatography(HPTLC)

Plants and plant-based products are the bases of many modern pharmaceuticals that are current in use today for various diseases.The aim of the study was to investigate the biochemical constituents and high performance thin layer chromatography（HPTLC） finger printing of the ethanolic extract of Evolvulus alsinoides.Phytochemical screening was done by standard procedures and HPTLC method was also established to analyze alkaloids,flavonoids and phenolic compounds from the ethanolic extract of Evolvulus alsinoides.Preliminary phytochemical screening showed that ethanol extracted more secondary metabolites than other solvents.HPTLC fingerprinting analysis showed the presence of various alkaloids,flavonoids and phenols（quercetin） in the ethanolic extract.It can be concluded that Evolvulus alsinoides may serve as a source of potent antioxidants that may be used in the prevention of various diseases such as cancer,diabetes and cardiovascular diseases due to the presence of phenolic compounds.HPTLC finger print of Evolvulus alsinoides may be useful in the differentiation of the species from adulterants and act as a biochemical marker for this medicinally important plant in the pharmaceutical industry and plant systematic studies.

六味能消丸TLC鉴别及3种蒽醌类成分的含量测定

目的建立六味能消丸的TLC鉴别方法,并采用一测多评法同时测定其中大黄素、大黄酚、大黄素甲醚的含量。方法采用TLC鉴别干姜、大黄药材。分析采用Phenomenex C_(18)色谱柱(150 mm×4.6 mm,5μm);流动相甲醇-0.2%H_(3)PO_(4)溶液(85∶15);体积流量1.0 mL/min;柱温30℃;检测波长254 nm。以大黄酚为内标,计算其他2种成分的相对校正因子,测定其含量。结果TLC斑点清晰,分离度良好。3种成分在各自范围内线性关系良好(r≥0.9998),平均加样回收率98.89%~101.11%,RSD 1.31%~1.69%。一测多评法所得结果与外标法接近。结论该方法准确稳定,重复性好,可用于六味能消丸的质量控制。

TLC-SERS同时检测降压类保健食品中五种沙坦类违禁添加成分

由于人们不健康的饮食结构和生活作息习惯以及人口老龄化等因素,高血压等慢性病发病率逐渐增高,降压类保健食品逐渐受到人们青睐。但是市场中存在不良商家为了提高保健食品的功效,向保健食品中非法添加降压药,尤其是沙坦类降压药的现象。建立了一种薄层色谱层析技术(TLC)与表面增强拉曼光谱(SERS)联用方法,对降压类保健食品中五种可能添加的沙坦类违禁成分(奥美沙坦酯、厄贝沙坦、氯沙坦钾、替米沙坦、缬沙坦)进行同步检测。对五种药物的SERS检测最佳条件进行探究,并通过比较不同成分及配比的TLC展开剂对于五种药物的分离效果,经过大量配方试验后成功得到环己烷-乙酸乙酯-甲醇-冰醋酸=53∶35∶12∶0.25(v/v/v/v)的分离体系,对五种药物具有良好的分离效果。确定实验条件后利用TLC分离技术对样品溶液分别进行初步分离,在薄层板上不同比移值的斑点原位处滴加金胶进行SERS检测,对样品溶液在斑点原位处的SERS光谱进行采集、比较,确定。研究结果表明,五种沙坦类违禁添加成分可通过TLC明确分离,且其SERS光谱特征峰一致、重复性良好,根据各自的特征峰可快速定性分析,检出限在0.1~1 mg·kg^(-1)之间。研究建立的TLC-SERS方法简单、快速,能够为保健食品中违禁添加成分的现场初步快速筛查提供一定参考。

TLC Identification and Extraction Process of Rubiasin-1-methyl Ether from Yao Medicine Chuanlianzhu

[Objectives]To establish a thin-layer chromatography(TLC)method for the determination of rubiadin-1-methyl ether in Yao Medicine Chuanlianzhu(Damnacanthus giganteus).[Methods]A silica gel G thin-layer plate was adopted for TLC.Petroleum ether(60-90℃)-chloroform-methanol-water(7:15:3:1)was used as the developing solvent and inspected under ultraviolet lamp(365 nm).The content was determined by Inertsil ODS-3 C 18 column(4.60 mm×250 mm,5μm),mobile phase:acetonitrile-0.2%phosphoric acid gradient elution,detection wavelength 277 nm,flow rate 1.0 mL/min,column temperature 30℃,injection volume 10μL.[Results]The spots of 10 Chuanlianzhu samples from different origins showed the same color at the same position as the control,and the spots were clear and specific.The injection volume of rubiadin-1-methyl ether showed a good linear relationship in the range of 2.90-145μg(R=0.9996).The average recovery rate of rubiadin-1-methyl ether in the low,medium and high dose groups of Yao Medicine Chuanlianzhu was 98.72%,and RSD=1.78%.[Conclusions]This method can effectively identify Yao Medicine Chuanlianzhu medicinal materials and accurately determine the content of rubiadin-1-methyl ether in the medicinal materials.It provides a scientific basis for the development and utilization of Yao Medicine Chuanlianzhu medicinal resources.

Simultaneous purification of minor components in natural products using twin-column recycling chromatography with a step solvent gradient

The isolation of minor components from complex natural product matrices presents a significant challenge in the field of purification science due to their low concentrations and the presence of structurally similar compounds.This study introduces an optimized twin-column recycling chromatography method for the efficient and simultaneous purification of these elusive constituents.By introducing water at a small flowing rate between the twin columns,a step solvent gradient is created,by which the leading edge of concentration band would migrate at a slower rate than the trailing edge as it flowing from the upstream to downstream column.Hence,the band broadening is counterbalanced,resulting in an enrichment effect for those minor components in separation process.Herein,two target substances,which showed similar peak position in high performance liquid chromatography(HPLC)and did not exceed 1.8%in crude paclitaxel were selected as target compounds for separation.By using the twin-column recycling chromatography with a step solvent gradient,a successful purification was achieved in getting the two with the purity almost 100%.We suggest this method is suitable for the separation of most components in natural produces,which shows higher precision and recovery rate compared with the common lab-operated separation ways for natural products(thin-layer chromatography and prep-HPLC).

Bio-screening and quantification of methyl paraben in vinegar and coconut juice separated by HPTLC

As a widely used food preservative,methyl paraben was experimentally evidenced with serious hormonelike adverse effects.Herein,a high performance thin-layer chromatography platformed bioluminescent bioautography and image analysis for the selective quantification and confirmation of methyl paraben was proposed and validated in vinegar and coconut juice.First,the detectability of the bioautography to the analyte on different layer materials was estimated,revealing that normal silica gel was the best choice.After that,the liquid of sample extract and working solution were separated to overcome the background noises due to co-extracted matrices.The separation result was then coupled to the optimized bioautography,enabling instant and straightforward screening of the targeted conpound.For accurate quantification,bioluninescent inhibition pattern caused by the analyte was processed by image analysis,giving useful sensitivity(LOD>16 mg/kg),precision(RSD<10.1%)and accuracy(spike-recovery rate 76.9%-112.2%).Finally,the suspected result was confirmed by determining its MS fingerprint,further strengthening the reliability of screening.

TLC Identification of Yao Medicine Pileostegia tomentellal and Extraction Technology and Content Determination of Umbelliferone

[Objectives]To establish a TLC and content determination method of Pileostegia tomentellal,with umbelliferone as the indicator component.[Methods]TLC identification was performed by silica gel G thin layer plate with n-hexane-ethyl acetate(4:3)as the developing agent,and the plate was examined by UV lamp(365 nm).The umbelliferone content was determined by HPLC:Inertsil ODS-3 C 18 column(4.60 mm×250 mm,5μm);mobile phase acetonitrile-0.2%phosphoric acid gradient elution;detection wavelength 320 nm,flow rate 1.0 mL/min,column temperature 30℃,injection volume 10μL.[Results]The chromatogram of P.tomentellal showed the same color spot in the same position as that of reference medicinal material,and the spot was clear with good specificity.Umbelliferone showed a good linear relationship when the injection volume was 2.63-131.27μg/mL(R^(2)=0.9997).The average recovery of umbelliferone in the low,middle and high adding groups of P.tomentellal was 99.57%and the RSD was 2.15%.[Conclusions]The method can effectively identify Yao medicine P.tomentellal and accurately determine the content of umbelliferone in medicinal materials,which will provide a scientific basis for the development and utilization of medicinal resources of Yao medicine P.tomentellal.

Determination of 14 Organophosphorus Pesticide Residues in Mutton by Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry(GPC-GC-MS)

[Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry(GC-MS)in selective ion scanning mode(SIM).[Results]The organophosphorus pesticide standard solutions showed good linearity in the mass concentration range of 0.1-10.0μg/ml with correlation coefficients(r)not lower than 0.999,and the detection limits(S=3 N)ranged from 0.01 to 0.05 mg/kg.The average recovery values were in the range of 80.2%-99.7%,with relative standard deviations(RSDs,n=3)in the range of 1.8%-6.3%,at the addition levels of 0.5,1.0 and 2.0 mg/kg.[Conclusions]The method is simple,sensitive and accurate,and can be used for the determination of organophosphorus pesticide residues in mutton.

Establishment of a TLC Identification Method for Ensete wilsonii

[Objectives]The paper was to establish a TLC identification method for Ensete wilsonii.[Methods]Usingβ-sitosterol as the reference,the effects of preparation methods of test solutions,developing solvents,developing distances and color developing agents on TLC analysis were investigated,and the best TLC conditions for E.wilsonii were determined.[Results]The test solution prepared with 90%methanol solvent was dotted on TLC silica gel G plate,and developed with dichloromethane-toluene-methanol=10:5:1.5 as the developing solvent.Then the plate was sprayed with 10%sulfuric acid ethanol solution,and dried with hot blast for color development.Finally,the plate was examined under an ultraviolet lamp at 365 nm.The TLC results of E.wilsonii obtained showed good separation and color development effect,and the spots were clear and characteristic.[Conclusions]This method is safe,specific,and easy to operate,and can be used as a TLC identification method for E.wilsonii.

Comprehensive analysis of phenolic composition and antioxidant mechanisms in Gymnema sylvestre extracts using LC-MS and column chromatography

Recent studies have highlighted the potential of plant extracts as therapeutic agents for managing oxidative stress and related disorders.This study aims to elucidate the phenolic composition and antioxidant properties of Gymnema sylvestre extracts.Ethanolic reflux extraction followed by column chromatography was employed to isolate phenolic compounds.The total phenolic and flavonoid contents were quantified using the Folin–Ciocalteu and aluminum chloride colorimetric methods,respectively.Antioxidant activities were assessed by DPPH,ABTS scavenging assays and the ferric reducing antioxidant power(FRAP)assay.High-Performance Liquid Chromatography(HPLC)with a C18 column and Thermo TSQ Quantum Access Max(LC-MS)were used to determine the levels of gymnemic acid and identify other potential phenolic compounds.The analysis revealed significant antioxidant activities in the fractions.Fraction A showed the highest DPPH and ABTS scavenging activities,and Fraction C demonstrated the highest ferric reducing power.LC-MS analysis identified several phenolic compounds,indicating that these are major contributors to the antioxidant efficacy of the extract.This study provides a detailed phenolic profile and confirms the strong antioxidant potential of Gymnema sylvestre leaf extract,supporting its therapeutic use and further investigation.

Determination of Benzo[a]pyrene in Edible Oil by High Performance Liquid Chromatography-Fluorescence Detector (HPLC-FL)

In this study, an optimized high performance liquid chromatography-fluorescence detector (HPLC-FL) method for the determination of benzo[a]pyrene in edible oil was established. HPLC was performed with Thermo Fisher Scientific C18 column (250 mm×4.6 mm, 5 μm) as the chromatographic column and acetonitrile and water as the mobile phase, and the excitation wavelength and emission wavelength of fluorescence detector were 286 and 430 nm, respectively. The response was high, and the linear range was 0.5-10.0 ng/ml. The lowest limit of detection was 0.11 ng/ml, and the average recovery was 92.5%. This method is suitable for quantitative analysis of benzo[a]pyrene content in edible oil.

Identification of Xunxi Shujin Decoction by TLC

[Objectives]To establish a TLC qualitative method for the determination of Radix Aconiti,Radix Aconiti Kusnezoffii,Caesalpinia sappan L.and Radix zanthoxyli.[Methods]TLC was used to study the quality of Radix Aconiti,Radix Aconiti Kusnezoffii and C.sappan L.in Xunxi Shujin Decoction,and the influencing factors were investigated to optimize the TLC conditions.[Results]In the TLC identification test of Radix Aconiti,Radix Aconiti Kusnezoffii,C.sappan L.and R.zanthoxyli in Xunxi Shujin Decoction,the spots were clear,the resolution was good,the specific value was moderate,the negative control was not disturbed,and the specificity was strong.[Conclusions]The established TLC method was simple,specific and reproducible,and could be used for the quality control of Xunxi Shujin Decoction.

牙膏中三七皂苷TLC定性检测法的改进

目的:寻找、建立一个磷酸氢钙与二氧化硅复配体系牙膏中三七皂苷检测薄层色谱的方法与规程,适用于检测、验证牙膏成品中含有三七根酊、三七花酊、三七总皂苷、三七叶皂苷。方法:以过滤、化学反应、萃取、吸附、洗脱等原理分离出牙膏中存在的三七根、叶、花皂苷,并制成供试样品,通过比较供试样品与对照样品在硅胶板上显现的点位,进行结果判断,确认该成品是否符合配方和生产工艺加工制出。结果:供试品与对照品以三氯甲烷-乙酸乙酯-甲醇-水(15∶40∶22∶10)为展开剂,5℃~10℃展开,喷以10%硫酸乙醇溶液显色,供试品中主要成分的色谱点,与对照品色谱点应显相同位置;置紫外光灯(365nm)下检视,显相同的荧光斑点。结论:通过本次方法学改进,确认符合磷酸氢钙与二氧化硅复配体系牙膏的TLC检测方法。

TLC插卡型模板早拆体系在施工中的应用

本文通过对TLC插卡型模板早拆体系在施工中的应用展开探讨,旨在分析技术应用效果以及优化应用策略,确保其技术效用的充分发挥。通过对相关文献的综合调研和分析,在施工现场使用TLC插卡型模板早拆体系,并结合实际案例探讨其应用流程。经过实践证明,TLC插卡型模板早拆体系能够显著提高施工效率。由于其设计先进,可灵活拆卸的特点,大大缩短了施工周期,节约了人力资源和材料费用。此外,该体系还具有较高的稳定性,能够有效防止模板的倾倒和坍塌等意外事故。综上所述,TLC插卡型模板早拆体系在施工中具有广阔的应用前景。为了充分发挥TLC插卡型模板早拆体系的优势,需要确保各环节施工作业的高效开展,这样一来才能够保障工程项目的整体建设效果。由此可见,在今后的建筑施工中,值得进一步推广和应用这种模板体系,以满足不断增长的建筑需求,推动建筑行业的健康可持续发展。

TLC插卡型模板早拆体系施工方法

文章立足于TLC插卡型模板特点,围绕该模板早拆体系的施工方法展开探讨,旨在进一步提高该模板体系的应用效率,为施工作业的高效开展奠定良好的基础。本文结合大量的文献资料,严格按照设计要求开展模板搭建、混凝土浇筑以及模板拆除等施工作业。TLC插卡型模板早拆体系的应用,应严格遵守相关标准要求,并对其进行科学优化和调整。研究结果表明,TLC插卡型模板早拆施工体系的应用,在缩短施工工期、提升施工效率等方面都发挥着非常关键的作用。而且该方法还具有可重复使用的特点,大大提升了建筑工程项目的节能环保效果,为后期建筑行业的健康可持续发展提供了可靠的保障。总之,TLC插卡型早拆体系使用方法值得在建筑工程项目建设中得到全面推广应用。希望通过本文的探究,能够为相关工作的开展起到参考作用。

TLC联合UPLC-QQQ-MS分析天王补心丸中4种外源性污染成分

目的对天王补心丸质量分析中发现的异常成分进行研究,建立薄层色谱(TLC)、超高效液相色谱—三重四极杆质谱(UPLC-QQQ-MS)同时测定天王补心丸中盐酸小檗碱、表小檗碱、盐酸黄连碱、盐酸巴马汀等4种外源性污染成分的分析方法。方法采用TLC法,通过优化展开系统,对158批样品进行定性鉴别;针对异常斑点,采用HPLC-Q/TOF-MS进行成分鉴定确认;采用UPLC-QQQ-MS进行定量分析。结果158批天王补心丸样品中有9批检出盐酸小檗碱、表小檗碱、盐酸黄连碱、盐酸巴马汀等4种外源性污染成分,分别在0.97~483.34、0.98~98.49、1.00~100.50、0.88~87.75ng·mL^(-1)内呈线性,回收率为99.30%~103.99%,平均标准偏差(RSD)为0.90%~2.62%(n=6),9批样品中上述4种成分的含量分别为20.3~104.1、1.0~17.6、0.4~30.6、3.2~24.8μg·g^(-1)。结论该方法简便、准确、专属性强,可为天王补心丸的质量控制提供参考。

TLC法鉴别复方氨酚烷胺片主成分

用薄层色谱法来鉴别复方氨酚烷胺片中的5种主成分,对原检验标准进行优化。以对乙酰氨基酚、马来酸氯苯那敏、咖啡因、盐酸金刚烷胺为对照品,采用硅胶GF_(254)薄层板,以三氯甲烷-甲醇-丙酮-氨水(9∶1.5∶1∶0.05)为展开剂,先在紫外光灯(254 nm)下检视,再喷以稀碘化铋钾显色剂;以胆酸、猪去氧胆酸为对照品,采用硅胶G薄层板,以乙酸乙酯-正己烷-甲醇-醋酸(25∶20∶3∶2)为展开剂,喷以10%硫酸乙醇溶液,105℃加热显色。改进的薄层色谱方法能有效分离4种主成分,显3个荧光斑点和两个色点;人工牛黄的薄层鉴别方法能定性胆酸和猪去氧胆酸。本方法结果准确,专属性强,薄层斑点清晰,分离度好,可替代原标准鉴别方法。

几种单糖、寡糖TLC条件的确立及草石蚕寡糖中水苏糖含量测定

目的:建立薄层色谱(TLC)分析几种单糖、寡糖的有效方法,并测定草石蚕寡糖中水苏糖含量。方法:以果糖、蔗糖、棉子糖和水苏糖为研究对象,从斑点分离度、斑点集中与否、有无拖尾现象及展开时间几方面探讨其在不同体系下的薄层色谱行为;通过薄层色谱扫描(TLCS)测定草石蚕寡糖中水苏糖含量。结果:确立适合的展开系统为乙酸乙酯/甲醇/水/冰乙酸(11.5:3.2:2:3.2),合适的显色剂为茴香醛-浓硫酸显色剂;草石蚕寡糖中水苏糖含量为69.3%。

应用TLC-FT-SERS对萝芙木中利血平成分的研究

本文报道了应用薄层色谱（ＴＬＣ） 与傅里叶变换表面增强拉曼光谱（ＦＴ－ＳＥＲＳ） 联用技术， 获得了中草药萝芙木有效成分利血平光谱研究的新方法。研究表明：在薄层原位约２ μｇ 的样品即可获得利血平分子的特征振动谱带，并阐述了样品分子在表面增强基底银微粒表面的吸附模式。

TLC和HPLC法相结合分析盐水鸭中的生物胺

应用薄层层析(TLC)和高效液相色谱(HPLC)两种方法分析盐水鸭中生物胺的组成及含量。薄层层析结果显示,盐水鸭样品中存在着腐胺、尸胺、亚精胺、精胺、酪胺和2-苯乙胺;利用高效液相色谱法也检测到了以上6种生物胺,且各生物胺的含量均在204μg/g以下。两种方法结果相吻合,TLC法可以作为肉制品中生物胺定性分析的一种经济便捷的方法。