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.

Study on Quality Standard of Corydalis tomentella Franch

[Objectives] To establish the quality standard of Corydalis tomentella Franch. [Methods] The medicinal materials are identified from the perspectives of morphology,characters,microscopic characteristics and TLC of the plants. The contents of moisture,total ash and water extract are determined. The content of dehydrocavidine is determined by HPLC. The determination is performed on Agilent C18 column with mobile phase consisted of acetonitrile-phosphate buffer solution( containing 20 mmol/L monopotassium phosphate,10 mmol/L diethylamine,0. 1% phosphoric acid)( 28∶ 72,V/V) at the flow rate of 1. 0 m L/min. The detection wavelength is set at 347 nm,and the column temperature is 35℃. The sample size is 10 μL. [Results] The original plants are perennial herbs,and as produced into medicinal materials,they are hairy and shrink into balls with conical principal roots,and obvious cracks on the tubers and roots,curved and fragmented leaves,yellowish white flowers. The quasi-circular pollen grains contain square and columnar crystals,there are substantial nonglandular hairs,and also bordered pits,spiral and reticulate vessels,as well as wood fibers. TLC spots are clear and well-separated. The content of moisture is7. 5%-18. 5%,total ash 20. 5%-26. 2%,and water extract 29. 9%-46. 4%. The linear range of dehydrocavidine is 0. 040 08-2. 404 8 μg( r =0. 999 9); RSD of precision,stability and reproducibility tests is lower than 2. 0%. The recoveries are 95. 6%-102. 5%( RSD =2. 3%,n = 9). [Conclusions] The established standard can be used for quality evaluation of C. tomentella Franch..

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.

Establishment of Quality Standard for Freeze-dried Tablets of Polygonatum sibiricum and Study on Anti-tumor Activity of Diosgenin

[Objectives]The paper was to establish the quality standard for freeze-dried tablets of Polygonatum sibiricum and to explore the antitumor activity of its extract diosgenin.[Methods]Taking freeze-dried powder samples of P.sibiricum from 4 different producing areas as materials,and referring to the quality standard of P.sibiricum in the Chinese Pharmacopoeia(2020 edition),the contents of total ash,moisture,extract,total sugar and diosgenin were determined by total ash determination method,drying method,hot dipping method,0.2%anthrone-sulfuric acid method and HPLC,respectively.The antitumor activities of diosgenin against A431(human epidermal carcinoma cells),H1975(human lung adenocarcinoma cells)and Ramos(human B lymphoblastoma cells)were investigated by MTT assay.[Results]The moisture content of the samples was 2.8%-4.7%(not more than 18.0%);the total ash content was 1.9%-3.4%(not more than 4.0%);the ethanol-soluble extract content was 72.99%-78.99%(not less than 45.0%);and the total sugar content was 7.95%-9.94%(not less than 7.0%).The lowest content of diosgenin was 0.18%,and diosgenin was significantly resistant to A431.[Conclusions]The content determination method established in the study is simple,accurate and reproducible.

Study on Preparation Process and Quality Standard of Tianlu Tongluo Granules

[Objectives]This study was conducted to optimize the preparation process of Tianlu Tongluo Granules and establish its quality standard.[Methods]Tianlu Tongluo Granules was prepared by an orthogonal test.TLC was used to identify Radix Astragali preparata,Radix Paeoniae Alba,Scutellariae Radix and Acori Tatarinowii Rhizoma in the granules,and the content of paeoniflorin in the finished product was determined by HPLC.[Results]The extraction process of Tianlu Tongluo Granules was as follows:adding 6 times of water,and decocting twice,1 h/time.In the forming process,the optimal ratio of thick paste to excipients as 10∶8.6,and the optimal ratio of excipients dextrin:starch:colloidal silicon dioxide was 6.5∶0.5∶1.6.The results showed that TLC spots were obvious,the separation was significant,and the specificity was strong.The paeoniflorin content had a good linear relationship in the concentration range of 5.9048-590.48 mg/L(r=0.9999).The average sample recovery was 101.10%,and the RSD was 1.18%.[Conclusions]The preparation process is stable and reasonable,and the established quality control method is specific and reproducible,and can be used for the quality control of Tianlu Tongluo Granules.

Research of Quality Standards for Stachydrine Hydrochloride in Chinese Medicine TJF Granule

A high-performance liquid chromatographic method was applied to the determination of stachydrine hydrochloride concentration in TJF granule (Chinese name: Tiao-Jing-Fang), using a mobile phase of methanol-acetonitrile (50:50, v/v) by the Agilent Kromasi NH2 column (250 mm × 4.6 mm, 5 μm, S/N: 22N25110). Detection wavelength was 201 nm. The result revealed good linearity of stachydrine hydrochloride and was obtained within the range of 0.20 - 1.98 μg/mL (R = 0.9995). The average recovery was 97.01%;the relative standard deviation (RSD) was 0.19%. To the best of our knowledge, this is the first report dedicated to the determination of stachydrine hydrochloride by the evaporative light scattering detector-high-performance liquid chromatographic (ELSD-HPLC) method.

Quality Standard of Qiang Herb Sophora davidii var.chuansiensis

[Objectives]To establish the quality standard of common clinical folk herb Sophora davidii var.chuansiensis.[Methods]The qualitative identification was performed by microscopic method and thin-layer chromatography(TLC).The contents of moisture,total ash,acid insoluble ash and extract were determined according to the methods of the Chinese Pharmacopoeia(2020).High performance liquid chromatography(HPLC)was used to determine the contents of oxymatrine and oxysophocarpine.[Results]The microscopic characteristics were obvious,including crystal sheath fiber,calcium oxalate square crystal,non glandular hair,stone cells,epidermal cells,stomata,cork cells,vessels with marginal pits and so on.TLC spots were clear,and the resolution was good.The contents of moisture,total ash,acid insoluble ash and extract from 10 batches of samples were 4.70%-8.33%,3.43%-4.19%,0.65%-1.02%and 14.67%-22.04%respectively.The determination results of oxymatrine were between 0.10%-0.33%,with an average value of 0.19%.The determination results of sophocarpine oxide were between 0.30%-0.38%,with an average value of 0.34%.[Conclusions]The established quality standard of S.davidii var.chuansiensis had good specificity and accuracy,and could be used for the quality control of herb S.davidii var.chuansiensis.

Development of Chuanxiong Toothpaste and Establishment of Its Quality Standard

The quality standard of Chuanxiong toothpaste was established.HPLC was used to determine the content of ferulic acid in Chuanxiong toothpaste and TLC was used to identify the Chuanxiong in the toothpaste.The content of active ingredients extracted from Traditional Chinese medicine by decocting water was high,and the corresponding toothpaste had a good hemostatic effect.The identification by use of thin layer chromatography(TLC)showed with clear spots and strong specificity for both the test product and the control product(Levistilide A)as observed under ultraviolet light(254 nm)with n-hexane-ethyl acetate(3∶1)as the developing agent,which could be used as the basis for the qualitative identification of Chuanxiong toothpaste.The ferulic acid in the range of 0.019,3~0.481,7μg mL^(-1) showed a good linear relationship with the peak area and the recovery rate of sample was between 99.5%and 101.2%.This method was simple,stable and reliable,and could be used as the quality control method for ferulic acid in Chuanxiong toothpaste.

药用辅料苯甲酸苄酯有关物质HPLC检测方法的建立

目的:建立苯甲酸苄酯有关物质的高效液相色谱方法,对该辅料质量标准提出修订建议。方法:用苯基硅烷键和硅胶为填充剂,以甲醇-1%-醋酸(60∶40)为流动相,检测波长为254 nm,流速1.0 mL·min^(-1),进样量20μL。结果:根据破坏试验结果,并兼顾分离度要求,确定了苯甲酸苄酯有关物质的色谱条件,并进行了方法学验证。有关物质中杂质苯甲酸和苯甲醛的检测限分别为0.2μg·mL^(-1)和0.01μg·mL^(-1),苯甲酸和苯甲醛的校正因子分别为1.0和0.1。按新建方法对4家企业6批次苯甲酸苄酯样品进行有关物质检查,均检出苯甲醛杂质,杂质含量在0.02%~0.1%。杂质总量在0.02%~0.9%。结论:新建立的方法可增订入苯甲酸苄酯的质量标准中,并根据给药途径的不同,制定不同的杂质限度,以便更好的控制药品质量。

RP—HPLC法同时测定白屈菜药材中血根碱、小檗碱和白屈菜红碱的含量

目的:建立白屈菜药材的质量标准。方法:采用高效液相色谱法,用 Diamonsil C_(18)色谱柱(250 mm×4.6 mm,5μm),以乙腈-1%三乙胺水溶液(25:75,三乙胺水溶液用磷酸调 pH 3)为流动相,流速:1 mL·min^(-1),检测波长263 nm,柱温:30℃。结果:血根碱在60～1200μg范围内线性良好,r=0.9996,平均加样回收率(n=3)为96.6%～99.9%,RSD 为0.6%～2.0%;小檗碱在30～600μg范围内线性良好,r=0.9999,平均加样回收率(n=3)为99.0%～104.1%,RSD 为0.8%～1.3%;白屈菜红碱在100～2000μg范围内线性良好,r=0.9998,平均加样回收率(n=3)为97.3%～100.8%,RSD 为0.7%～1 4%。结论:本试验同时测定白屈菜药材中血根碱、小檗碱、白屈菜红碱的含量,方法准确,灵敏,可靠。

杯装速溶奶茶中含茶成分HPLC检测及其质量标准与饮用安全性的研究

在合肥大型超市中选取8款不同品牌杯装速溶奶茶产品,参照GB/T 8313-2008儿茶素HPLC检测方法,改进样品前处理方法,利用无水乙醇对样品进行超声波辅助提取,测定奶茶样品中主要含茶成分儿茶素和咖啡碱的含量。结果表明,8款品牌的杯装速溶奶茶均符合GB/T 21733-2008《茶饮料》中奶茶饮料中茶多酚和咖啡碱的含量要求。研究结果为杯装速溶奶茶中主要含茶成分的测定提供了一种参考方法。还对杯装速溶奶茶的质量标准、奶茶饮用安全性进行了探讨。

愈银片的HPLC指纹图谱研究

目的:建立愈银片的高效液相色谱(HPLC)指纹图谱。方法:采用HPLC法。色谱柱为Inertsil ODS-3,流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为230 nm,柱温为30℃,进样量为10μL。以槲皮素为参照物,测定10批愈银片的HPLC图谱,采用《中药色谱指纹图谱相似度评价系统》(2012版)进行共有峰指认和相似度评价。结果:10批愈银片的HPLC图谱有39个共有峰,相似度均>0.96。经验证,10批样品HPLC图谱与对照指纹图谱具有较好的一致性。结论:该研究所建指纹图谱可为愈银片的鉴别和质量评价提供参考。

HPLC法测定不同部位、不同产地桔梗中党参炔苷的含量

目的采用HPLC法测定不同部位、不同产地桔梗中党参炔苷含量,为补充桔梗质量评价标准提供参考。方法色谱柱为Introject C18（250 mm×4.6 mm,5μm）,以乙腈和水为流动相进行梯度洗脱,流速为1.0 ml/min,检测波长267 nm,柱温30℃。结果党参炔苷在0.065 625~1.05 g/L（R2=0.999 1）范围内与峰面积呈良好线性关系,精密度良好,平均回收率为98.41%。不同部位、不同产地桔梗药材中党参炔苷的含量范围为0.031 5~0.489 9 mg/g。结论不同部位、不同产地的桔梗药材中党参炔苷的含量差异较大;本法准确可行、重复性好,可以用于桔梗及其制品中党参炔苷的含量检测。

基于HPLC指纹图谱及多元功效成分定量分析的南五味子药材质量标准提升研究

目的:建立不同产地南五味子药材HPLC指纹图谱及多元功效成分定量分析方法,为南五味子药材质量标准提升提供支撑。方法:采用HPLC,以乙腈-0.1%甲酸水为流动相,梯度洗脱,建立南五味子药材指纹图谱,并以7个木脂素类成分为测定指标建立南五味子药材含量测定方法。结果:建立了南五味子药材HPLC指纹图谱,标定了28个共有峰,并鉴定了其中7个峰;各样品图谱与对照图谱相似度均大于0.93。所测定的7个成分在测定浓度范围内线性关系良好,平均加样回收率为97.4%~99.2%,RSD均小于3.0%。结论:南五味子药材的指纹图谱特征性和专属性强,结合木脂素类成分的测定,可为全面控制南五味子药材的质量提供科学方法。

HPLC法测定前列通颗粒中盐酸小檗碱的含量

目的建立HPLC法测定前列通颗粒中盐酸小檗碱的含量。方法采用Phenomenex Luna C18色谱柱(4.6 mm×250 mm,5μm),流动相:乙腈-0.01 mol/L磷酸(40∶60),检测波长:346 nm,柱温:40℃,流速:1.0 ml/min。结果盐酸小檗碱回归方程为Y=2496.028X-57.420,r=0.9999,表明盐酸小檗碱在0.09～0.45 mg范围内具有良好的线性关系;平均回收率为99.76%,RSD为0.85%。结论本法稳定可靠,可作为前列通颗粒的含量测定方法。

HPLC法同时测定四黄止痛喷雾剂中黄芩苷、小檗碱和大黄素的含量

目的:建立同时测定四黄止痛喷雾剂中3种有效成分黄芩苷、小檗碱与大黄素的含量的HPLC法。方法:采用安捷伦ZORBAX SB-Aq色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈(A)-0.05 mol/L磷酸二氢钾溶液(用磷酸调节p H至3.0)(B),采用梯度洗脱(0~9 min,24%A;9~10 min,24%A→29%A;10~20 min,29%A;20~22 min,29%A→63%A;22~32 min,63%A),流速为1.0 m L/min,柱温为30℃,检测波长分别为280 nm(黄芩苷),265 nm(盐酸小檗碱),254 nm(大黄素)。结果:黄芩苷、盐酸小檗碱和大黄素进样量分别在0.5907~2.9536μg(r=0.9999),0.3046~1.5232μg(r=1),0.01444~0.0722μg(r=1)范围内线性关系良好;加样回收率(n=6)分别为99.86%、100.84%和99.66%,RSD分别为1.24%、1.97%和1.35%。结论:本法适用于同时测定四黄止痛喷雾剂中黄芩苷、盐酸小檗碱和大黄素的含量。结论:该方法简便、准确、重复性好,可为制定四黄止痛喷雾剂质量标准及产品质量控制提供依据。

HPLC法测定利肝隆冲剂中五味子醇甲的含量

目的 :修订利肝隆冲剂的质量标准。方法 :用HPLC法测定五味子醇甲的含量。结果 :五味子醇甲在 0 .0 8～ 1.2 0 μg范围内呈良好的线性关系 :r=0 .9991,平均回收率 99.3% ,RSD为 1.1%。结论 :所建立的方法简便可行 ,重现性好 ,为利肝隆冲剂质量控制提供了方法。

HPLC测定黄连提取物中生物碱含量

目的 建立黄连提取物高效液相色谱法（HPLC）含量测定方法.方法 采用HPLC同时测定黄连提取物中表小檗碱、黄连碱、巴马汀、小檗碱等生物碱的含量.色谱柱为Kromasil 100-5 C18,流动相为乙腈-磷酸盐缓冲液（53：47,v/v）,流速为1 mL/min,检测波长为345 nm,进样量为10 μL.结果 盐酸小檗碱在0.1032～2.5800 μg范围内进样量与其峰面积线性关系良好（r=0.9999,n=7）,平均回收率为100.19％（RSD=1.77％）.测定6批黄连提取物,其中表小檗碱、黄连碱、巴马汀、小檗碱含量分别不少于5.5％,11.5％,9.0％,44.0％,总生物碱含量不少于70.0％.结论 本文建立含量测定方法简便可行,准确、重现性好,可用于黄连提取物的质量控制.

HPLC-ELSD测定三七胶囊中人参皂苷Rg_1和Rb_1

目的 :研究三七胶囊的质量标准。方法 :应用HPLC ELSD对三七胶囊中的活性成分人参皂苷Rg1和Rb1的含量进行测定。结果 :人参皂苷Rg1在 1.3 μg～ 6.5μg范围内呈现良好的线性关系 (r =0 .9994) ,平均回收率为 98.3 0 % ,RSD为 1.2 0 % (n =5)。人参皂苷Rb1在 1.0 μg～ 5.0 μg范围内呈现良好的线性关系 (r =0 .9996) ,平均回收率为 97.12 % ,RSD为 1.17% (n =5)。结论 :该方法简便 ,快速 ,重现性好 。