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 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.

ANALYSIS OF HUMAN PLACENTA BY ^(31)P NUCLEAR MAGNETIC RESONANCE AND THIN-LAYER CHROMATOGRAPHY SCANNING COMBINED WITH THE CORRECTIVE METHOD OF ABSORBANCE PROPORTIONAL COEFFICIENT

Five phospholipids in human placenta were determined by phosphorus 31 nuclear magnetic resonance(^(31)P NMR)spectroscopy and thin-layer chromatography(TLC) scanning combined with the corrective method of absorbance proportional coefficient. The NMR spectrometer used this investigation was a Bruker AM-500 spectrometer operating at 202.4 MHz for ^(31)P chemical shifts are relative to 85% phosphoric acid. TIC was carried out by silica gel H plate developed in chloroform-methanol-glacial acetic acid-ethanol-water(25:4:6:2:0.5),with Vaskovsky reagent as colour -developing agent of phospholipids.

Quality Evaluation of Leontopodium franchetii Beauv. from Different Localities Based on Moisture,Ash and Extract Contents and Thin-layer Chromatography

[Objectives] The aim was to determine the moisture,ash and extract contents in Leontopodium franchetii Beauv. from different localities. [Methods] The contents of moisture,total ash,acid-insoluble ash and extract in L. franchetii from different localities were determined according to the methods described in Chinese Pharmacopoeia( 2015 Edition). [Results] In the 10 samples,the contents of moisture were all less than or equal to 15. 0%; the contents of total ash were all below 12. 0%; and the contents of acid-insoluble ash were all less than 3. 0%. The contents of water-soluble extract( by cold-soaked extraction method) in the samples were all below 12. 0% except those from Hongyuan Prairie of Sichuan Province and Xinglong Mountain in Lanzhou City,Gansu Province. [Conclusions]The contents of the four indicators measured in this experiment varied by small margins,indicating that the quality was relatively stable. This study provides theoretical data for the revision of the quality standards for L. franchetii.

Separation of Amino Acids Based on Thin-Layer Chromatography by a Novel Quinazoline Based Anti-Microbial Agent

A newly designed quinazoline based compound, 6-pyridin-2-yl-5,6-dihydro-benzo[4,5]imidazo[1,2-c] quinazoline (PDBIQ) has shown the ability for the easy detection of nineteen amino acids on thin-layer chromatography plates as a spray reagent. This new reagent enabled to produce various distinguishable colors with amino acids with different RF values. The detection limits and the binding ability of PDBIQ with amino acids have been calculated. PDBIQ is also able to detect aminoacids from hydrolised seed protein. The title compound also exhibited profound inhibitory action against some gm (+ve) and gm (-ve) bacterial organisms. This paper deals with synthesis, spectroscopic application and biological evaluation of the organic moity.

Preparation Process and Thin Layer Chromatography Identification of Wufang Babu Poultice

[Objectives] To establish the process flow of preparation of Wufang Babu Poultice and the identification method of thin layer chromatography (TLC). [Methods] For the forming process of Wufang Babu Poultice, the preparation method of mixed pharmaceutical powder with suitable pharmaceutical excipients was adopted. Qualitative identification of medicinal materials in Wufang Babu Poultice (Strychni Semen, Rhei Radix Et Rhizoma, Dipsaci Radix, and Angelicae Sinensis Radix) was carried out by TLC. [Results] Mixed pharmaceutical powder mixed with glycerol, gelatin and other pharmaceutical excipients can be prepared for forming. The test solution chromatography of each medicinal material (Strychni Semen, Rhei Radix et Rhizoma, Dipsaci Radix, Angelicae Sinensis Radix) showed pigment spots of the same color at the same position as its corresponding control medicinal materials and reference chromatography, and the display was clear. [Conclusions] The preparation process is simple and feasible, and can be used as the forming process of Wufang Babu Poultice. The TLC determination method is simple to operate, has good specificity, and has no effect on negative results, and can be used for identification of Wufang Babu Poultice.

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。

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。

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。

Separation of liquefied product of Salix psammophila by column chromatography and structure analysis of its components

The liquefied product of Salixpsammophila wood was separated by thin-layer chromatography （TLC） and column chromatography, and its structure was identified by nuclear magnetic resonance （NMR） spectra in our study. The separation result indicates that the sample of liquefied S. psammophila contained at least two categories of components. The structure of the main components was guaiacyl C-1, C-2 of the hydroxyphenyl propane, i.e., the aromatic nucleus protons of lignin. Degradation and polycondensation reactions occurred when the S. psammophila wood was liquefied in phenol. Polycondensation reactions occurred among the depolymerization products from cellulose, the aromatic depolymerization products from lignin and the products of the displacement reactions between phenoxide ion and cellulose.

TLC-分光光度法测贯叶连翘中金丝桃素含量

:针对贯叶连翘中成分复杂 ,干扰物多的特点 ,采用薄层层析 (TL C)分离出金丝桃素后 ,再进行分光光度测定。薄层层析以石油醚 -乙酸乙酯 -甲醇 (1∶ 4∶ 3)为展开体系展开 ,金丝桃素的 Rf=0 .85。分光光度法测定的回归方程为 A=72 .0 0 C+0 .0 0 3(r=0 .9997) ,平均回收率为 97.9% (RSD=0 .87% )。

TLC-HPLC检测三黄连合剂的有效成分

【目的】以薄层色谱法—高效液相色谱法（TLC-HPLC）检测三黄连合剂的有效成分,为制定其质量标准及后期临床推广应用提供理论依据。【方法】采用TLC对三黄连合剂中的主要组分黄连、黄芩和连翘进行定性鉴别,并以HPLC对其主要有效成分黄芩苷、盐酸小檗碱和连翘苷进行含量测定。【结果】三黄连合剂TLC色谱中的图像斑点清晰,与标准品对照斑点对齐,颜色一致。HPLC测定三黄连合剂中黄芩苷、连翘苷和盐酸小檗碱分别在75.00-1200.00μg/m L（r=0.9997）、4.17-66.67μg/m L（r=0.9998）、9.38-150.00μg/m L（r=0.9999）范围内线性关系良好,平均回收率分别为113.92%、100.18%和100.40%,其含量分别为5.03、0.25和0.27 mg/m L。【结论】TLC-HPLC可作为三黄连合剂的质量控制方法,且操作简便、重现性良好。

基于薄层色谱与一测多评法的沙棘颗粒质量评价方法研究

目的:优化中成药沙棘颗粒的薄层鉴别方法,建立多成分高效液相色谱一测多评方法。方法:采用薄层色谱法对槲皮素、异鼠李素和山柰素进行定性鉴别;采用高效液相色谱法,C18色谱柱(250 mm×4.6 mm,5µm),流动相为乙腈-0.1%磷酸水溶液,梯度洗脱,流速为1.0 mL·min^(–1),柱温为35℃,检测波长为365 nm,以槲皮素为内参物计算异鼠李素和山柰素含量。结果:薄层色谱鉴别方法斑点清晰、专属性好;与外标法对比,一测多评法准确度高、耐用性好。结论:优化的薄层色谱法与建立的一测多评法可靠、准确、重复性好,可为沙棘颗粒的质量标准提升提供参考。

TLC-生物自显影-MTT法检测滇重楼内生真菌中抗菌活性成分

本文采用TLC-生物自显影-MTT法检测了3株滇重楼内生真菌即芬芳镰刀菌、季氏毕赤氏酵母和烟曲霉正丁醇提取物对大肠杆菌、枯草芽孢杆菌、白色念珠菌和稻瘟病菌的抗菌活性成分,以芬芳镰刀菌和季氏毕赤氏酵母菌液提取物中含有的抗菌活性成分为多。同时与打孔药剂扩散法的检测结果进行了比较,为进一步快速分离内生真菌中抗菌活性成分提供了依据。

大蒜中低聚糖的TLC鉴别和HPLC-RID含量测定

目的建立大蒜中低聚糖的薄层色谱(TLC)法和高效液相-示差折光检测器(HPLC-RID)法,用于大蒜中低聚糖的鉴别和含量测定。方法采用TLC法大蒜中果糖、蔗糖、蔗果三糖和蔗果四糖进行鉴别,以冰乙酸-氯仿-水(21/18/4)为展开系统,苯胺-二苯胺溶液为显色剂;采用HPLC-RID法测定大蒜中果糖、蔗糖、蔗果三糖和蔗果四糖的含量,色谱柱为碳水化合物分析柱(4.6×250 mm,4μm);流动相:乙腈-水(75/25),柱温:35℃,流速:1.0 mL/min,进样量:15μL。结果薄层色谱中可以检测到果糖、蔗糖、蔗果三糖和蔗果四糖4种低聚糖。果糖、蔗糖、蔗果三糖和蔗果四糖分别在0.03~0.81、0.5~16.04、0.02~0.65、0.02~0.64 mg/mL范围线性关系良好。4种糖类低、中、高浓度平均回收率(n=3)分别为98.0%、99.7%、100.3%和98.2%;测定新疆5种不同海拔(1733、1680、1250、2800、2300 m)大蒜中果糖、蔗糖、蔗果三糖、蔗果四糖的含量分别为0.34~0.54、6.54~8.74、0.45~0.61、0.04~0.15 mg/g。结论本研究建立的大蒜中低聚糖的定性、定量分析方法准确可靠、重现性好,可用于大蒜中低聚糖的鉴别和含量测定。

黎药弯柄灵芝质量标准初步研究

目的:初步建立黎药弯柄灵芝的质量标准。方法:对弯柄灵芝药材的性状进行鉴定,对其显微特征进行鉴别;参照《中国药典》2020年版方法,采用薄层色谱法(TLC)对药材进行定性鉴别,采用分光光度法测定药材中的多糖和三萜及甾醇含量。结果:明确了弯柄灵芝的性状及显微特征,建立了专属的TLC定性鉴别法;初步规定了弯柄灵芝多糖含量不得低于0.80%,三萜及甾醇含量不得低于0.90%。结论:本研究建立的弯柄灵芝药材质量标准可为其质量控制及资源可持续利用提供依据。

关于TLC/FID法测定误差的探讨

TLC/FID法分析重质油中的烃族组成,具有灵敏、快速、用样量少的优点;但过去一直存在着与经典柱色谱法所测数据可比性差的致命缺点。为此,从TLC分离及FID检测的基本原理出发,寻找合适的操作条件,使两种方法具有良好的相关性,完成了TLC/FID法由半定量向定量分析的转变。欲减少误差.提高准确度,关键是要做好以下几点:①严格控制点样量,以保证数据重复性;②选择适宜的TLC展开条件,以保证被测定物质各组分的分高效果;③控制适宜的扫描速度和氢气流量等操作条件;④用被测定物质各组分校正因子的比值进行数据处理,确保测定结果的准确性。

红麻花甲醇可溶性色素TLC分离与成分鉴定

以红麻花为原料,通过对红麻花甲醇可溶性色素的薄板层析(TLC)分离研究,得到其TLC最佳展层剂是:V(乙酸乙酯)∶V(水)∶V(甲酸)∶V(乙酸)=70∶30∶3∶2。以最佳展层剂展开花中的色素,得到4条颜色深浅不一的色带,反映该花色素至少含4种色素单体成分。对色素母液及第一单体成分样液进行290～700 nm扫描测定表明,色素母液在253.9 nm及372.6 nm各有一特征吸收峰;色素第一单体样液的特征吸收峰在252.7 nm及369.0 nm。初步鉴定结果揭示:红麻花甲醇可溶性色素成分主要为黄酮醇类。

六味能消制剂中非法成分土大黄苷检测方法的建立

目的建立六味能消丸(胶囊、片)中非法成分土大黄苷的检测方法。方法用薄层色谱法及高效液相色谱-二极管阵列检测器法初步筛查样品中非法成分土大黄苷,并用高效液相色谱-串联质谱法对土大黄苷检测阳性结果进一步进行确证。结果在101批次六味能消丸(胶囊、片)中的12批次六味能消丸中检出土大黄苷。结论所建立的方法专属性强,可有效筛查六味能消制剂中是否含有土大黄苷。

败酱草质量研究

目的:建立败酱草的薄层鉴别方法(TLC)及HPLC测定东莨菪内酯含量测定方法,为败酱草的质量研究提供依据。方法:采用TLC鉴别法,HPLC作为含量测定方法,色谱柱:Ultimate Plus C_(18)(4.6 mm×250 mm,5μm);流动相:乙腈-0.5%冰醋酸(15∶85);柱温:25℃;流速:1 mL·min^(-1);检测波长:343 nm。结果:薄层鉴别中检出与对照药材相同颜色的荧光斑点;东莨菪内酯在0.8384~20.96μg·mL^(-1)范围内线性关系良好(函数关系为Y=39.233X+7.0215,r=0.9999),回收率为91.0%~97.9%,均值为95.4%,RSD(n=6)为3%。结论:本方法鉴别专属性较好,含量测定方法专属性、稳定性、重现性、准确度良好,可用于败酱草的质量控制。