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.

Multiple Chromatographic and Chemometric Methods for Quality Standardization of Chinese Herbal Medicines

Quality standardization of complementary medicine is fundamental for industry and practice as it underpins the quality,safety and efficacy of Chinese herbal medicines.Current herbal standardizations are often based on the quantitative analysis of a single compound,which may not reflect the total characteristic,bioactive and toxic nature of the herbs or products.Therefore,there is a need to establish an internationally recognized methodology for quality standardization of Chinese herbal medicines.The analytical methods reviewed in this article are pharmacognosy,TLC,HPLC,LCMS,CE and chemo-metrics.This article also covers the developments and applications of these methods in quality standardization.Recent advances show that a combination of these methods creates an overall chemical profile of each herb.This is supported by results reviewed in this article and obtained in our laboratory tests on medicinal herbs including Hypericum perforatum,Morinda officinalis and Centella asiatica.Significant variations in active components have been observed between herbal samples and products.It is proposed that the identification of active components,pharmacological activities and eventual clinical applications are required for a comprehensive quality standardization system.Our findings indicate that the combination of various chromatographic and chemometric methods will advance the methodology of quality standardization and enhance the overall confidence in herbal medicine for the health practitioner and the public.

Study of Cuscuta chinensis Lam. in Nuhuang Fuzheng Oral Liquid by Thin Layer Chromatography

[Objectives] To better control the quality of Nuhuang Fuzheng Oral Liquid and study the main component Cuscuta chinensis Lam.by Thin Layer Chromatography. [Methods] Through changing the treatment methods of the test sample solution,proportion of the developing solvent and sample application volume,taking the spot resolution,definition,and Rf value,optimal Thin Layer Chromatography conditions were screened for Cuscuta chinensis Lam. [Results] After the test sample solution passing the neutral alumina column,it was extracted two times using the ethyl acetate. Methanol was added to dissolve. Benzene-ethyl acetate-formic acid( 5∶5∶2.5) was used as developing solvent.And ammonia fumigation was carried out to develop color. In the thin layer chromatograph obtained through these conditions,Nuhuang Fuzheng Oral Liquid test sample solution showed the same stripe in the same position of the control drug chromatogram and there was no obvious tailing phenomenon and the spot was clear. [Conclusions] The thin layer chromatography identification conditions can be used as the method for quality control of Cuscuta chinensis Lam. in Nuhuang Fuzheng Oral Liquid.

Identification of Ethnic Medicine Polygonum capitatum by Thin Layer Chromatography

[Objectives]To establish a thin-layer chromatography identification method for the ethnic medicinal materials of Polygonum capitatum.[Methods]The thin layer chromatography(TLC)method was used to identify materials.[Results]The TLC identification showed that in the chromatogram of the test sample,there were spots of the same color in the corresponding position of the chromatogram of the reference medicinal material,and the reproducibility was good.[Conclusions]The TLC identification and the determination results of the inspection items can provide a basis for the quality control of the medicinal materials of P.capitatum.

Identification of Citric Acid in Wuhuang Oral Liquid by Thin Layer Chromatography

[Objectives] To screen the identification conditions of citric acid in Wuhuang Oral Liquid by thin layer chromatography,and establish the quality control method for citric acid in Wuhuang Oral Liquid.[Methods] Different treatment methods were adopted for test sample,developing agent,and drying time,thin layer chromatography separation condition and spot definition were taken as indicators to conduct experiment,to select optimal thin layer identification method. [Results] Methanol was used as the extraction solvent,ultrasonic treatment,ether extraction,dissolution by anhydrous ethanol as treatment conditions of test sample; upper solution of butyl acetate-formic acid-water(4 ∶ 2 ∶ 2) after placing one hour was taken as developing agent; 0. 1% bromocresol green(BCG) as the developer; when developing the color in 3 hours after development,in thin layer chromatograph,there appeared the same strip in the same position of test sample of Wuhuang ORAL Liquid and control substance,no obvious trailing phenomenon,and the color was uniform and clear.[Conclusions]The thin layer chromatography identification conditions can be used as the method for quality control of Wuhuang Oral Liquid.

Study on Quality Standards of Jianjin Zhuanggu Paste

[Objectives]Some Chinese medicinal materials of Jianjin Zhuanggu Paste were microscopically identified,and several active ingredients were studied by thin-layer identification,which provides reference for further improving the quality standards of hospital preparations.[Methods]The effective components of Jianjin Zhuanggu Paste were qualitatively identified by thin-layer chromatography(TLC).[Results]The microscopic identification of the three Chinese medicinal materials in Jianjin Zhuanggu Paste showed the microscopic characteristics of Radix Codonopsis,Radix Astragali and Radix Notoginseng.TLC identification showed that there were characteristic spots of Radix Codonopsis,Radix Astragali,Radix Rehmanniae Preparata and Radix Notoginseng in Jianjin Zhuanggu Paste.[Conclusions]This study established the quality standard research method of Jianjin Zhuanggu Paste,which further strengthens the safety standards of hospital preparations,and improves the clinical efficacy of drugs,as well as the quality standards of hospital preparations to a certain extent.

Study on Quality Standards of Laportea bulbifera(Sieb. et Zucc.) Wedd. in Yao’s Folk-medicine

[Objectives] This study was conducted to establish the quality control standards for Laportea bulbifera(Sieb. et Zucc.) Wedd. [Methods] Microscopic identification and thin layer chromatography were used to identify and determine the moisture, total ash and extract contents. [Results] According to the microscopic results, the stem transection is round and has five longitudinal edges at which the cell wall is obviously thickened. Bristles can be observed. A series of collenchyma cells are arranged closely inside the epidermis. There are several rows of parenchyma cells. The vascular bundles are of different sizes;and the ray part is wide, and at the junction of the ray and the cortex, there are often scattered secretory cells. The center is a broad medulla. The powder is brown. There are many starch grains. The bristles are unicelluar, and have warty protrusions and expanded base. The fibers are bundled, and the cells are large. The epidermal cells are in the shape of an elongated spindle, in a mosaic arrangement, and the cell wall is slightly thickened. From the thin layer identification chromatograms of tested L. bulbifera, it can be seen that spots were observed at the same positions as the control medicinal material, and the durability of the method was good. The extract content should not be less than 12.00% by hot extraction with water as solvent, and not be less than 3.00% by cold extraction with ethanol as solvent. The moisture content should not be more than 16.50%. The total ash content should not be more than 14.00%. The acid-insoluble ash content should not be more than 2.50%. [Conclusions] The microscopic identification results are reliable and can be used as the identification basis of L. bulbifera. The thin layer identification method and the test results can provide a basis for quality control of L. bulbifera.

Study on Quality Evaluation and Standards of the Zhuang Medicine Pandanus tectorius Soland.

[Objectives] This study was conducted to establish the quality control standards for Pandanus tectorius Soland.[Methods] Microscopic identification and thin layer chromatography were used to identify and determine the moisture,total ash and extract contents.[Results] The root transection is near round.The outmost side is velamen.There are nearly 10 columns of collenchyma tissue cells inside.In the cortex,there are a large number of fiber bundles scattered,and there are also large mucous cells scattered.The endodermis is distinct,and the cells are small and closely arranged.The pericycle is distinct and forms a ring.The pericycle fiber bundles are arranged in a radial shape by more than 40 bundles of phloem and xylem alternately.The leaf transection is V-shaped.The collenchyma lies under the epidermis.The spongy tissue has many calcium oxalate square crystal and needle crystals.The mucous cells contain calcium oxalate square crystal and needle crystals.The thin layer identification indicated that in the chromatogram of each test sample,spots of the same colors appeared at the positions corresponding to the chromatogram of the reference medicinal material,and the reproducibility was good.The moisture contents of the 10 batches of samples were all below 8.0%.The total ash was below 8.0%.The acid-insoluble ash was below 2.0%.With 50% ethanol as the solvent,the extract contents were all over 12.5%.[Conclusions] The microscopic identification results are reliable and can be used as the identification basis of P.tectorius.The thin layer identification method and the test results can provide a basis for quality control of P.tectorius.

Study on Quality Standards of Children Antipyretic Lotion

[Objectives]To establish suitable quality standards of children antipyretic lotion.[Methods]Qualitative identification was performed for Paederia scandens and Artemisia carvifolia in Children Antipyretic Lotion by thin-layer chromatography(TLC),and the content of paederosidic acid in children antipyretic lotion was determined by high performance liquid chromatography(HPLC).Besides,chromatographic column Feinigen XPeonyx C18(250 mm×4.6 mm,5μm),mobile phase was used,gradient elution was carried out with acetonitrile-0.1%phosphoric acid aqueous solution,the detection wavelength was 236 nm,the flow rate was 1.0 mL/min,the column temperature was 30℃,and the injection volume was 10μL.[Results]The thin-layer chromatography of P.scandens and A.carvifolia reference materials showed clear spots,good separation effect,strong specificity,and no interference in the limit control;paederosidic acid showed a good linear relationship in the range of 0.65-9.75μg(R2=0.9996),the average sample recovery rate was 99.72%(RSD=2.52%).[Conclusions]The qualitative and quantitative methods established in this experiment are simple,reproducible,and the results are accurate and reliable,and can be applied as a quality control method for children antipyretic lotions.

Quality Standard of Compound Quanchangning Capsule

[ Objective] The research aimed to study the quality standard of Compound Quanchangning Capsule. [ Method] Coptis, Phelledendron, Pulsatilla and Astragalus in Compound Quanchangning Capsule were indentified qualitatively by thin layer chromatography （ TLC）, and the content of berberine hydrochloride was determined by high performance liquid chromatography （HPLC）, to study the quality standard of Compound Quanchangning Capsule. [ Result] TLC identification showed that the tested product was clear and well-separated with no interference. Berberine hydrechloride showed a good linear relationship with peak area at the injection volume of 10.92 - 163.74 ~Lg/mL, and the regression equation was Y = 39 611X -2 387. 9 （R2 = 0. 999 8） ; the average recovery was 97.60%, and the relative standard deviation was 1.64% （n =6）. [ Conclusion] The standard is simple in operation and good in specificity, stability and repeatability, which is prompted as a favorable method for quality control of Compound Quanchangning Capsule.

Establishment of Quality Standard for Mongolian Medicines Shoushen and Naishoushen

[Objectives] To systematically identify and analyze pharmacognostical features of Mongolian medicine Shoushen and Naishoushen( dairy tablets) to provide scientific basis for the establishment and identification of its quality standard. [Methods] According to relevant methods specified in Appendix to 2010 Chinese Pharmacopoeia,the water content,total ash,and extracts of Shoushen and Naishoushen were detected,and thin layer chromatography( TLC) was applied to make qualitative identification. Gastrodin was used as the reference substance,extracted with 70% methanol,and then sprayed with ethyl acetate-formic acid-water( 9∶ 1∶ 0. 2) as the developing solvent,and then sprayed with 10% phosphomolybdic acid ethanol solution and heated at 105℃ to clear spot color. UV-Visible spectrophotometry and high performance liquid chromatography( HPLC) were used to analyze the content of polysaccharides and gastrodins in Shoushen and Naishoushen. The chromatographic column was a ZOBB AX eclipse XDB-C_(18)( 4. 6 mm × 250 mm,5 cm) column with the methanol-0. 04% phosphoric acid solution( 8∶92) as the mobile phase,the flow rate of 1. 0mL/min,the detection wavelength of 222 nm,and the column temperature of 30℃.[Results]In the thin-layer chromatography test,spots of the same color appeared at the positions corresponding to the chromatogram of the reference substance. Gastrodin eluted under high pressure reached baseline separation. Gastrodin had a good linearity in the concentration range of 0. 009-0. 09 mg/m L. The regression equation was Y = 586 866 X + 425 821( R^2= 0. 999 6),and the average recovery rate was100. 1%. Precision test,reproducibility test,and stability test conformed to the requirements. The results of extracts of three batches of samples were 26. 13%-42. 58%,water content was 3. 47%-5. 31%,and total ash was 5. 43%-6. 33%. [Conclusions] The quality control method has high reliability,high sensitivity,high specificity,high accuracy,and high stability. The results are expected to provide a scientific basis for the identification,resource utilization,and improvement of quality standard for Shoushen and Naishoushen.

Study on quality standard of Danmu exract syrup

Objective:To establish the quality standard of Danmu exract syrup.Methods:TLC method was used to qualitatively identify Nauclea officinalis in Danmu exract syrup.The content of strictosamide and chlorogenic acid in Danmu exract syrup was determined by high efficiency axillary chromatography.Results:The spots were clear and there was no negative interference.The linear relationship of strictosamide was good in the range of 100~300ug/ml(R^(2)=0.9997).The average recovery was 99.1%and RSD was 1.16%(n=9).Chlorogenic acid had a good linear relationship in the range of 6.7~20.2ug/ml(R^(2)=0.9991).The average recovery was 99.9%and RSD was 1.10%(n=9).Conclusion:The standard is safe and reasonable,the method is simple,accurate and reproducible,and it can be used for the quality control of Danmu exract syrup.

Study on Quality Standard of Lujing Yiqi Shengxue Pills

[Objectives]This study was conducted to establish the quality standard for Lujing Yiqi Shengxue Pills to provide a basis for its quality control.[Methods]According to the quality requirements in the 2020 edition of Chinese Pharmacopoeia,the quality of Lujing Yiqi Shengxue Pills was evaluated from the aspects of properties,identification,inspection and content determination.Radix Astragali,Radix Angelicae Sinensis,Macrocephalae Rhizoma stir-fried with bran and Radix Paeoniae Alba in the preparation were identified and studied by thin layer chromatography(TLC).A high performance liquid chromatography(HPLC)method was established to determine the content of paeoniflorin in the preparation.[Results]The thin layer spots of Radix Astragali,Radix Angelicae Sinensis,Macrocephalae Rhizoma and Radix Paeoniae Alba were clear and round,and the negative preparations had no interference.The properties,moisture,weight difference,loading difference,dissolution time limit and microbial limit all met the requirements.The regression formula for the quantitative analysis of paeoniflorin in the concentration range of 4.86-194.40μg/ml was:Y=12.0241X+0.8797,R^(2)=0.9999;and the average recovery was 98.9%,and the RSD was 1.7%.[Conclusions]The method has good repeatability,and is stable,feasible,simple and convenient in operation and suitable for quality control of Lujing Yiqi Shengxue Pills.

Quality Control of Zhuang Medicine Xiaoyan Zhiyang Lotion

[Objectives]To establish the TLC identification methods of Llicis Rotundae Cortex and Mahoniae Caulis and the determination method of syringin content in Zhuang Medicine Xiaoyan Zhiyang Lotion.[Methods]Thin layer chromatography(TLC)was used to qualitatively identify Llicis Rotundae Cortex and Mahoniae Caulis in Zhuang Medicine Xiaoyan Zhiyang Lotion.The quantitative analysis of syringin in Zhuang Medicine Xiaoyan Zhiyang Lotion was carried out by high-performance liquid chromatography(HPLC).Chromatographic conditions are as follows:Luna 5μm C_(18)((2)100 A(250 mm×4.6 mm,5μm)column was adopted;acetonitrile(10%)-water(90%)was as the mobile phase,and the flow rate was 1.0 mL/min;the detection wavelength was 265 nm;the sample size was 5μL;the column temperature was 30℃.[Results]Syringin had a good linear relationship with its peak area in the range of 0.190-2.856μg(R^(2)=0.9995).The RSD values of precision,stability and repeatability experiments were all lower than 2.5%,and the average sampling recovery rate(n=6)was 100.37%(RSD=-0.88%).[Conclusions]The method had the advantages of simple operation,strong specificity,good repeatability and stability,and can be used for the quality control of Zhuang Medicine Xiaoyan Zhiyang Lotion.

前列桂芍颗粒质量标准研究

目的制定前列桂芍颗粒质量标准。方法采用薄层色谱法(TLC)对前列桂芍颗粒中熟地黄、赤芍、桃仁、黄芪、黄柏进行定性鉴别;通过使用高效液相色谱法(HPLC)测定盐酸小檗碱在前列桂芍颗粒中的含量。结果前列桂芍颗粒中薄层色谱鉴别专属性强,斑点清晰且阴性无干扰;前列桂芍颗粒中盐酸小檗碱的线性范围是0.0901~1.6215μg(r=0.9998),平均回收率为98.54%,RSD值为0.87%(n=6)。结论薄层色谱鉴别和含量测定方法准确可行,重复性好,可有效控制前列桂芍颗粒质量。

宠物用丹参咀嚼片制备工艺研究及质量标准建立

旨在确定宠物用丹参咀嚼片的制备工艺并建立其质量标准。本试验通过湿法制粒辅料种类、制粒工艺、压片工艺进行考察,确定其制备工艺,采用薄层色谱法、高效液相色谱法(HPLC)对宠物用丹参咀嚼片中丹参酮ⅡA、丹酚酸B分别开展定性和定量研究,建立其质量标准。结果:将丹参喷雾粉加辅料混合均匀,混合时间5 min,转速100 r/min,以10%淀粉浆为黏合剂制成颗粒,干燥温度40~50℃,0.3%硬脂酸镁作为润滑剂,压片速率10~35 r/min;薄层鉴别显示丹参酮ⅡA斑点清晰,分离度良好且专属性强;高效液相色谱显示丹酚酸B在8.0~256.0μg/mL范围内线性关系良好(R^(2)=0.999 9),系统适用性、专属性、精密度、稳定性、重复性、系统耐用性良好,加样回收率为95.0%~105.0%;对6批样品中丹酚酸B进行含量测定,设定含量限度为11.484 1 mg/g。综上,本试验确定的宠物用丹参咀嚼片制备工艺稳定可行,建立的薄层鉴别方法和高效液相色谱含量测定方法可用于宠物用丹参咀嚼片的质量控制。

益肝片的质量标准研究

目的:提升益肝片的质量标准。方法:采用薄层色谱法(TLC)鉴别益肝片中的板蓝根、虎杖;采用高效液相色谱法(HPLC)对益肝片中的(R,S)-告依春和大黄素进行含量测定。结果:通过TLC鉴别板蓝根、虎杖,相应斑点清晰、分离度好,阴性无干扰。(R,S)-告依春在进样量0.03~0.15μg范围内与峰面积线性关系良好(r=0.9998),平均加样回收率为97.05%,大黄素在进样量0.0495~0.297μg范围内与峰面积线性关系良好(r=1.0000),平均加样回收率为99.24%。结论:本质量标准能有效鉴别益肝片中的板蓝根、虎杖,也能有效测定(R,S)-告依春和大黄素的含量,且该法简便、可靠、重复性好,可用于益肝片的质量控制。

芪归养血颗粒质控标准研究

目的研究建立芪归养血颗粒质控的标准。方法采用薄层色谱法(TLC)对黄芪、淫羊藿、菟丝子进行定性鉴别,通过超高效液相色谱-蒸发光散射检测器(UPLC-ELSD)测定制剂中黄芪甲苷含量:色谱柱:Acclaim RSLC 120 C_(18)(100 mm×2.1 mm,2.2µm),ELSD,流动相为乙腈-水(32∶68),流速为0.4 ml/min;柱温30℃;进样体积为1μl。结果TLC能特异性鉴别黄芪、淫羊藿、菟丝子。黄芪甲苷的注射量与峰面积具有良好的线性关系,线性范围为0.0826~0.8260µg,r=0.9996;平均回收率为99.19%,相对标准偏差(RSD)为0.74%。结论采用TLC法和UPLC-ELSD检测对芪归养血颗粒分别进行了定性鉴别和定量分析,所建立的方法专属性强,结果准确,可作为芪归养血颗粒的质控方法进行应用。

蒙药地格达-8味散的定性定量方法研究

目的:建立蒙药地格达-8味散定性定量方法,为地格达-8味散的质量控制提供依据。方法:采用薄层色谱法对地格达-8味散中木香、黄柏、肋柱花、胡黄连、麦冬等5种处方药进行定性研究;采用高效液相色谱法测定地格达-8味散中獐芽菜苦苷、盐酸黄柏碱、胡黄连苷Ⅱ、木犀草苷、胡黄连苷Ⅰ、盐酸小檗碱、木香烃内酯和去氢木香内酯等8种成分研究。结果:TLC条件下,供试品色谱中在与相应对照品、对照药材色谱相应的位置上,显相同颜色的斑点、Rf值适宜,阴性对照无干扰。地格达-8味散中獐牙菜苦苷、盐酸黄柏碱、胡黄连苷Ⅱ、木犀草苷、胡黄连苷Ⅰ、盐酸小檗碱、木香烃内酯、去氢木香内酯平均回收率分别为98.8%、97.5%、98.4%、98.6%、97.8%、99.1%、98.1%和98.6%,平均含量为0.121%、0.022%、0.056%、0.019%、0.045%、0.077%、0.013%、0.018%。结论:建立的蒙药地格达-8味散质量控制方法专属性强,准确度高,操作简便,可用于地格达-8味散的质量控制。

黄连琥珀清心丸质量标准研究

为了建立黄连琥珀清心丸的定性定量检测方法,并为后续建立其质量标准提供依据,对方中的沉香、广枣、诃子、黄连、木棉花、肉豆蔻6味药进行显微鉴别;对诃子进行薄层鉴别;使用高效液相色谱法(HPLC)对盐酸小檗碱进行质量分数测定。建立了黄连琥珀清心丸的显微鉴别、薄层鉴别,方中盐酸小檗碱在0.0180~0.9020 mg/mL范围内呈良好的线性关系,质量分数检测方法科学、灵敏、重复性好,精密度、稳定性、重复性试验中相对标准偏差均小于3.0%,加样回收实验平均回收率为101.29%,相对标准偏差为2.30%,所建立的质量标准操作简便、重复性好,可用于黄连琥珀清心丸的质量标准研究。