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.

Extraction Process and Quality Standard of Danshen Jianxin Capsules

[Objectives]This study was conducted to establish the quality standard of Danshen Jianxin Capsules.[Methods]Orthogonal design was adopted to optimize the water extraction process by taking the amount of water added,extraction time and extraction times as factors,and the content of tanshinone I as the index.Salviae Miltiorrhizae,Notoginseng Radix Et Rhizoma and Radix Astragali in the capsules were qualitatively identified by TLC,and the content of tanshinone I in the capsules was determined by HPLC.[Results]The best water extraction process included the steps of adding 12 times of water each time,extracting the materials twice,for 1 h each time.In TLC identification,the test samples showed spots of the same color at the positions corresponding to tanshinone II A,ginsenoside Rg1,notoginsenoside R1 and astragaloside IV reference samples.[Conclusions]Danshen Jianxin Capsules was prepared by the water extraction method,which is characterized by high efficiency and being suitable for mass production.The quality control method is reliable,fast and accurate,which can effectively control the quality of the product.

Study on Quality Standard of Zhuang Medicine Buddlejae Flos

[Objectives]This study was conducted to explore the quality control method and establish the quality standard of Zhuang medicine Buddlejae Flos.[Methods]The microscopic identification method was adopted to identify the characters and microscopic characteristics of dried Buddlejae Flos in combination with traditional experience.The moisture,ash,acid-insoluble components and extracts of Buddlejae Flos were determined with reference to general rules of Chinese Pharmacopoeia(2015 edition).TLC identification was performed.Liquid chromatography-mass spectrometry(LC-MS)was used to determine the contents of linarin and verbascoside in Buddlejae Flos,and gas chromatography-mass spectrometry(GC-MS)was adopted to detect pesticide residues in Buddlejae Flos.Heavy metal elements As,Cd and Pb were detected by inductively coupled plasma mass spectrometry(ICP-MS).[Results]The established method is simple and accurate.Clear spots were observed on the thin layer chromatograms,and the resolution was good.The average value of moisture content was 12.24%;the average value of ash content was 5.1%;the average value of acid-insoluble content was 7.5%;and the average value of extract content was 27.3%.The regression equation of rutin in Buddlejae Flos was y=11.896x-0.0049,R^(2)=0.9996,and the contents of linarin and verbascoside were 5680 and 2080 mg/kg,respectively.No pesticide residues and heavy metals were detected in the medicinal materials of Buddlejae Flos.[Conclusions]This study can provide reference for the quality standard control of Guangxi Zhuang medicine Buddlejae Flos.

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.

Quality Standards of Carpesium lipskyi

[Objectives]The paper was to establish the quality standard of Carpesium lipskyi,and to provide a scientific reference for its quality control and rational development and utilization.[Methods]Morphological identification,microscopic identification and thin layer chromatography(TLC)identification of the herbal samples were performed.The contents of moisture,total ash,acid-insoluble ash and alcohol-soluble extract of the herbal samples were determined,and their total flavonoid content was determined by UV-spectrophotometry.[Results]The average contents of moisture,total ash,acid-insoluble ash and alcohol-soluble extracts of 10 batches of C.lipskyi were 10.38%-12.27%,8.03%-14.72%,1.01%-3.06%and 20.84%-26.82%,respectively.The total flavonoids content ranged from 4.60%to 5.63%.[Conclusions]The established standard can provide a reference for the quality control of C.lipskyi.The tentative regulations stipulate that the moisture content of C.lipskyi shall not exceed 13.0%;the total ash content shall not exceed 15.0%;the acid-insoluble ash content shall not exceed 4.0%;the alcohol-soluble extract shall not be less than 16.0%;and the total flavonoids shall not be less than 3.0%.

Quality Standard of Oxyria sinensis Hemsl

[Objectives]To establish the quality standard of Oxyria sinensis Hemsl.[Methods]The method in Chinese Pharmacopoeia(2020 edition)was used to determine the moisture,total ash,acid-insoluble ash and alcohol-soluble extracts of O.sinensis.The qualitative identification of medicinal materials was carried out by microscopic identification method and thin layer chromatography(TLC).The contents of hyperoside and isoquercitrin were determined by high performance liquid chromatography(HPLC).[Results]The total amount of moisture,total ash,acid-insoluble ash,alcohol-soluble extract,hyperoside and isoquercitrin of 12 batches of medicinal materials were 8.56%-11.53%,11.26%-15.48%,1.62%-2.56%,17.75%-26.09%,and 0.036%-0.42%,respectively.The microscopic features were obvious,and pores,fibers,calcium oxalate clusters,calcium oxalate square crystals,cork cells could be observed.Fluorescent spots of the same color were displayed at the positions corresponding to the hyperoside reference substance.[Conclusions]Establishing relatively complete quality standards for O.sinensis medicinal materials can provide a reference for the quality control of medicinal materials.

Quality Standard Research of Shenqi Qiangjing Granules

[Objectives]The paper was to establish the quality standard of Shenqi Qiangjing granules and to conduct routine inspection of granular dosage forms.[Methods]The particle size,moisture,loss on drying,dissolubility,content uniformity and microbial limit of Shenqi Qiangjing granules were detected.Radix Astragali,Herba Epimedii,Radix Dipsaci and Fructus Schisandrae Chinensis were qualitatively identified by thin layer chromatography(TLC).[Results]The particle size,moisture,loss on drying,dissolubility,content uniformity and microbial limit of Shenqi Qiangjing granules were all in line with the relevant regulations of Pharmacopoeia of the People's Republic of China(2020 edition).Radix Astragali,Herba Epimedii,Radix Dipsaci and Fructus Schisandrae Chinensis had clear fluorescent spots in TLC assay,and no such spots were found in negative control.[Conclusions]The method has the advantages of simple operation,accurate and reliable results,strong specificity and good repeatability,and can effectively control the quality of Shenqi Qiangjing granules.

The development of Fructus corni quality standard considering the effects of processing

The quality standards for Fructus Comi have been established based on the effects of the manufacturing processes.Three critical process parameters(CPPs)of extraction,filtration,and concentration to prepare Fructus Comi concentrate were identified by Plackett-Burman design with a single batch of Fructus Corni,which were heating medium temperature,extraction time,and water addition.Morroniside yield,loganin yield,and dry matter yield were process critical quality attributes(CQAs).CPPs arranged with a Box-Behnken design were applied to treat different batches of Fructus Comi After constructing a model that included CPPs,material propertie s,and process CQAs,loganin content was found to be the critical material attribute(CMA).The design space was calculated with a probability method.According to the limits of process CQAs,the minimum content of loganin in Fructus Corni was calculated with an error propagation method,which was 6.92 mg·g^(-1).When the content of loganin in Fructus Corni reaches up to 6.92 mg·g^(-1),the material is considered high-quality and is most suitable for the process.High-quality material can be used for production of Fructus Comi concentrate.This method can also be used to set material quality standards for other Chinese medicines.

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.

First Forum on China Casting Quality Standards & Overview of Revision History of China's National/Industrial Standards for Foundry Operations

Both national and local governments have been paying great attention to the work of industrial standardization with the enormous increase in international trade after China joined WTO. According to the standards revising plan of Standardization Administration Committee of China (SAC),TC54 has already revised a series of national standards and industrial standards for foundry operations,and proposed some new ones. As a result,some old fashioned standards containing low-level techniques have been gradually discontinued or replaced with new versions.……

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 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..

Preliminary Study on Formulating Water Quality Standards for Estuaries of China

In China,the water quality standards in operation include the Environmental Quality Standard for Surface Water（GB3838-2002）and Water Quality Standards for Seawater（GB3097-1997）.However,these two standards are currently not suitable for the estuarial zones of China because of the unique properties of water environment in estuaries.We proposed preliminarily a basic idea and technical workflow in formulating water quality standards for the estuaries of China based on analyzing the water environment properties of estuaries comprehensively and comparing various parameters and their standard values mentioned in these two standards above.Issues pertinent to the formulation of the water quality standards for estuaries,e.g.nutrient,heavy metals and persistent organic pollutants（POPs）,are highly concerned.The objective of this paper is to provide technical support for the formulation of scientific water quality standards and the assessment of water quality of the estuaries of China.

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.

Quality standard study of Li folk medicine callicarpa nudiflora powder

Objective:To establish the quality standard of Li folk medicine callicarpa nudiflora powder by modern analytical method.Methods:TLC was used to identify the powder.Five heavy metals and harmful elements(Pb,Cd,As,Hg and Cu)in the powder were determined by flame atomic absorption spectrometry and hydride atomic fluorescence spectrometry.The content of luteolin and Mullein glycoside in the powder was determined by HPLC.Results:the fluorescent spots of TLC identification of powder were clear,and the separation of the two main components was good.It has good specificity,reproducibility and durability,which can be used for the identification of the powder.The inspection items of heavy metals for the identification of powder were established.It was stipulated that:according to the determination method,the lead should not exceed 5 mg/kg;the cadmium should not exceed 0.3 mg/kg;the arsenic should not exceed 2 mg/kg;the mercury should not exceed 0.2 mg/kg;the copper should not exceed 20 mg/kg.The content of luteolin and Mullein glycoside in the powder were determined by HPLC and the content inspection item of the powder was established.It was stipulated that the content of luteolin and Mullein glycoside in the powder should not be less than 0.48%and 5.83%,which can be used for the content limit inspection of the powder.Conclusion:the quality standard method established by our institute is advanced and operable,and can be used for the quality control of the powder.

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.

Study on the preparation and quality standard of Callicarpa nudiflora film

Objective:To screen the best prescription and technology of Callicarpa nudiflora film,and to study and establish the quality standard of the flim.Methods:The orthogonal test was used to investigate the effect of PVA content,glycerin content,ethanol and water ratio on the comprehensive score of the coating agent;the general inspection method and content determination method were used to control the quality of Callicarpa nudiflora film,and the quality standard of the film was established.Results:The best formulation was selected as polyvinyl alcohol 6.0g,glycerin 2ml,ethanol:water 1:1.The appearance,stability,heat and cold resistance of the film were good,and the quality standard of the film was established.Conclusion:The formulation is simple and feasible,and the quality control method of the film is stable and feasible.

Development of emergency water quality standard for Cr^(6+) and Hg^(2+) in Liao River basin

The acute toxicity data of Cr＋ and Hg2＋ to the aquatic organisms in Liao River basin was collected and screened. Calculated results of criteria values using popular species sensitivity distribution （SSD） methods were evaluated through data analysis. The comprehensive methodology of emergency water quality standards （EWQSs） was established on the basis of the SSD method of Australia and New Zealand according to the evalu- ation results. The affected fractions of the aquatic organisms were set to be 5 %, 15 %, 30 % and 50 %, corre- sponding to the risk grades of Ⅰ,Ⅱ,Ⅲ and IV, and four-grade EWQSs, respectively. The EWQSs for Cr6＋ and Hg2. in the Liao River were derived and the corresponding risk indicators were also proposed. The results showed that the four-grade EWQSs for Cr6＋ were 2.85 μg/L, 21.0 μg/L, 161 μg/L and 797 μ/L, respec- tively, and the risk indicators were daphnia （grade Ⅱ ）, shrimp （grade Ⅲ）, and the bighead fish or tadpole （grade IV）. The four-grade EWQSs for Hg2＋ were 0.59 μg/L, 2.32 μg/L, 6.25 μg/L and 15.6 μg/L, respective- ly, and the risk indicators were crucian carp or daphnia （grade Ⅱ）, shrimp （grade Ⅲ）, and worm or crab （grade IV）. The results provided valuable information for the risk analysis of sudden ambient water environmen- tal pollution accident.