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。

Ten-year observation of corneal densitometry and associated factors following small incision lenticule extraction

●AIM:To investigate the long-term changes of corneal densitometry(CD)and its contributing elements after small incision lenticule extraction(SMILE).●METHODS:Totally 31 eyes of 31 patients with mean spherical equivalent of-6.46±1.50 D and mean age 28.23±7.38y were enrolled.Full-scale examinations were conducted on all patients preoperatively and during followup.Visual acuity,manifest refraction,axial length,corneal thickness,corneal higher-order aberrations,and CD were evaluated.●RESULTS:All surgeries were completed successfully without complications or adverse events.Ten-year safety index was 1.17±0.20 and efficacy 1.04±0.28.CD value of 0–6 mm zones in central layer was statistically significantly lower 10y postoperatively,compared with preoperative values(0–2 mmΔ=-1.62,2–6 mmΔ=-1.24,P<0.01).There were no correlations between CD values and factors evaluated.●CONCLUSION:SMILE is a safe and efficient procedure for myopia on a long-term basis.CD values get lower 10y postoperatively,whose mechanism is to be further discussed.

Early changes in corneal densitometry after FS-LASIK combined with accelerated corneal cross-linking for correction of high myopia

AIM:To observe the effects of femtosecond laserassisted excimer laser in situ keratomileusis combined with accelerated corneal cross-linking(FS-LASIK Xtra)on corneal densitometry after correcting for high myopia.METHODS:In this prospectively study,130 patients underwent FS-LASIK or FS-LASIK Xtra for high myopia.Their right eyes were selected for inclusion in the study,of which 65 cases of 65 eyes in the FS-LASIK group,65 patients with 65 eyes in the FS-LASIK Xtra group.Patients were evaluated for corneal densitometry at 1,3,and 6mo postoperatively using Pentacam Scheimpflug imaging.RESULTS:Preoperative differences in corneal densitometry between the FS-LASIK and FS-LASIK Xtra groups in different ranges were not statistically significant(P>0.05).Layer-by-layer analysis revealed statistically significant differences in the anterior(120μm),central,and total layer corneal densitometry between the FS-LASIK and FS-LASIK Xtra groups at 1 and 3mo postoperatively(all P<0.05),the FS-LASIK Xtra group is higher than that of the FS-LASIK group.Analysis of different diameter ranges showed statistically significant differences between the FS-LASIK group and the FS-LASIK Xtra group at 1mo postoperatively in the ranges of 0–2,2–6,and 6–10 mm(both P<0.05);At 3mo postoperatively,the FS-LASIK Xtra group is higher than that of the FS-LASIK group in the ranges of 0–2 and 2–6 mm(P<0.05).At 6mo postoperatively,there were no statistically significant differences in corneal densitometry between the FS-LASIK group and the FS-LASIK Xtra group in different diameter ranges(all P>0.05).CONCLUSION:There is an increase in internal corneal densitometry during the early postoperative period after FS-LASIK Xtra for correction of high myopia.However,the densitometry values decreased to the level of conventional FS-LASIK at 6mo after surgery,with the most significant changes observed in the superficial central zone.

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.

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.

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.

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。

小蓟TLC鉴别方法优化及小蓟炭“炒炭存性”内在表征研究

目的优化小蓟TLC鉴别方法并研究小蓟炭“炒炭存性”内在表征。方法对2020年版《中国药典》中“小蓟”项下TLC展开方法中的薄层板和展开剂进行改进,建立小蓟炭的TLC鉴别方法和UPLC指纹图谱,并测定蒙花苷、金合欢素的含量。结果小蓟TLC鉴别建议使用硅胶G板,展开剂建议改为甲苯-丙酮-甲酸-甲醇(6∶3∶0.5∶2.5)。小蓟及不同炒制程度小蓟炭的蒙花苷、金合欢素含量变化与TLC鉴别结果一致。结论与2020年版《中国药典》相比,改进的小蓟TLC鉴别方法较原方法成本低,所用展开剂毒性小。建立的小蓟炭“炒炭存性”的内在表征结合外观性状可用于解决市售小蓟炭的质量问题。

基于茚三酮衍生化TLC-SERS检测血清中的多巴胺

基于茚三酮衍生化薄层色谱法(TLC)与表面增强拉曼光谱法(SERS)联用传感技术建立了一种简便、灵敏度高和选择性高的血清中多巴胺的分离检测方法。多巴胺与茚三酮的橘红色衍生化产物不仅带来可视化效果,而且提供了良好的SERS响应,大大增强了SERS强度。薄层色谱法是一种快速有效的分离方法,表面增强拉曼光谱法具有灵敏度高,能够直接给出分子信息的特点,实现了一种无标记且无损的衍生化TLC-SERS传感检测方法用于检测血清中的多巴胺。

Quantitative Estimation of Gallic Acid as Biomarker in Lipitame Tablets by HPTLC Densitometry for Diabetic Dyslipidemia

Lipitame is a poly herbal formulation comprised of Terminalia arjuna, Terminalia belerica, Commiphora mukul and Phyllanthus emblica. The formulation is investigated for its analysis evaluation. Biomarkers of three herbs such as Terminalia arjuna, Terminalia belerica, and Phyllanthus emblica have been already cited to contain gallic acid, which was qualitatively and quantitatively estimated. In the present study rapid and inexpensive qualification methods for the quality control of Terminalia arjuna, Terminalia belerica, Commiphora mukul and Phyllanthus emblica on thin layer chromatography (TLC) were developed and validated. The solvent system used was toluene:ethyl acetate:formic acid:methanol (12:9:4:0.5). The scanning of plate was performed linearly at 273 nm (absorption) by use of a TLC Scanner III CAMAG with a deuterium source, and the area of spots corresponding to Gallic acid standard was integrated. It was found that gallic acid has been found in the Lipitame tablets on HPTLC densitometry assessment compared with authentic gallic acid reference standard.

TLC-SERS对鸡肉中的氧氟沙星快检研究

采用薄层色谱法与表面增强拉曼光谱联用技术(TLC-SERS)分离和检测鸡肉中的氧氟沙星(OFX)。薄层色谱法(TLC)可以将目标分析物从混合物中快速分离出来,解决了SERS无法准确识别目标分析物的问题,且SERS具有灵敏无损的特点。采用商用硅胶60 F254荧光板作为固定相,无需对样品进行预处理,将含有OFX的鸡肉组织液混合液滴在商用硅胶板上即可实现TLC分离。鸡肉混合样品采用TLC分离后,在OFX对应位置滴加银纳米粒子,采用银纳米粒子作为增强基底,进行SERS检测。TLC-SERS联用技术实现了快速分离检测鸡肉的氧氟沙星,其检出限可达到0.01 ppm。

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。

蒙药钦汤散质量标准的优化与提升

目的:优化与提升蒙药制剂钦汤散的质量标准。方法:采用薄层色谱(thin layer chromatography,TLC)法对钦汤散中五灵脂和红花进行定性鉴别;采用高效液相色谱(high performance liquid chromatography,HPLC)法测定穗花衫双黄酮的含量,色谱条件为C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸水(66∶34),柱温为25℃,检测波长为330 nm,流速为1.0 mL/min。结果:TLC法结果显示,供试品在与对照品或对照药材色谱图相应位置上显示相同颜色斑点,且阴性对照无干扰,专属性强;HPLC法结果显示,穗花衫双黄酮峰面积在12.0~21.6μg/mL范围线性关系良好,回归方程为y=119894x-253379(R^(2)=0.9993);高中低加样回收率试验,平均回收率为104.5%、102.9%、103.5%,RSD为1.15%、1.63%、0.28%;穗花衫双黄酮含量在0.01284%~0.01293%区间范围内。结论:本研究所建立的蒙药钦汤散的鉴别和含量测定方法准确可靠,灵敏度高、重复性好、精密度高和专属性强,可以用于优化与提升蒙药制剂钦汤散的质量标准。

TLC插卡型早拆模板体系在装配式施工中的应用

TLC插卡型早拆模板体系,在实际施工过程中,凭借着安装操作难度低,安装快捷,施工安全有保证,并且凭借早拆体系特有的优势,可以提高材料的周转效率,与装配式结构施工配合使用,更可以有效的加快施工进度,降低成本。其施工难度低,满足施工规范需求,也可以减少施工管理成本,不论在经济效益或社会效益方面,都值得进一步推广。本文对该早拆模板体系在实际施工中的操作及重点进行详细论述。

复方中药提取液中何首乌和参须的TLC鉴别分析

研究以何首乌和参须为对照药材的复方中药提取液质量标准的制定。方法 根据最佳提取工艺,提取何首乌、参须、阴性对照复方中药药材以及完整复方中药药材的主要成分。查阅并筛选《中华人民共和国药典》 (2015年版)一部的相关项,选取最适合的薄层色谱法,对何首乌和参须的大黄素型蒽醌和人参皂苷进行定性分析,同时进一步筛选薄层色谱法的展开条件,优化完整复方中药提取液的薄层鉴别条件。预期结果 实现最大程度提取出有效成分,在筛选得到薄层色谱法最佳展开和显色条件中大黄素型蒽醌和人参皂苷的斑点清晰可见,分离度符合要求,无阴性干扰。结论 本文设计的何首乌和参须主要成分大黄素型蒽醌和人参皂苷的提取工艺和薄层色谱法定性鉴别方法简便易操作,结合了科学理论和传统经验,专属性和准确性高,可作为何首乌和参须的质量标准控制方法。

金水六君煎物质基准中半夏和陈皮的薄层鉴别研究

目的:建立经典名方金水六君煎物质基准中半夏和陈皮的薄层鉴别方法。方法:以半夏对照药材为对照,对金水六君煎中半夏进行薄层鉴别研究,以橙皮苷和陈皮对照药材为对照,对金水六君煎中陈皮进行薄层鉴别研究,并对其进行方法学验证。结果:建立的薄层色谱法能鉴别出半夏和陈皮,斑点对应较好,阴性无干扰,方法学考察结果显示,方法适应性良好。结论:本法简单可行、结果可靠、重复性好,可作为金水六君煎物质基准的质量控制方法。

接骨丹片质量标准提升研究

目的 提升接骨丹片的质量标准。方法 采用薄层色谱法鉴别制剂中的制马钱子和大黄;采用高效液相色谱法同时测定马钱子碱和士的宁的含量,色谱柱为Kromasil 100-5-C_(18)柱(250 mm×4.6 cm,5μm),流动相为乙腈-0.01 mol/L庚烷磺酸钠与0.02 mol/L磷酸二氢钾等量混合溶液进行梯度洗脱,流速为1.0 mL/min,检测波长为260 nm,柱温为30℃,进样量为10μL。结果 制马钱子、大黄的薄层色谱图斑点清晰,分离度高,且阴性对照无干扰。马钱子碱和士的宁的质量浓度分别在1.46~116.73μg/mL和1.60~128.30μg/mL范围内与峰面积线性关系良好(r=0.999 5,0.999 7,n=6);精密度、重复性、稳定性试验结果的RSD均小于2.0%(n=6);平均加样回收率分别为97.28%和96.23%,RSD分别为1.16%和1.36%(n=6)。结论 该方法专属性好,结果准确、可靠,可用于接骨丹片的质量评价。